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### 1 

## PART VII . SUMMARY OF TEST PROCEDURES, METHODS, AND REPORTING REQUIREMENTS FOR DISTILLATION FEED COMPOSITION ANALYSIS

The EPA petroleum refinery test progr am is requesting variability data for the feed to the distillation column. This part provides an overview 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 requested include: mercury, chlorine, sulfur, antimony, arsenic, beryllium, cadmium, chromium, cobalt, lead, manganese, nickel, and selenium

.
You will need to collect triplicate 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 results 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, preparing, and analyzing the distillation feed samples are outlined below.

Note: If you have multiple distillation columns and the feed to each is similar ( i.e. , the feed to one distillation column is representative of the feed 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 example, if you have three 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 are 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 pa rt 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 th at 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 distilla tion 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). Deleted: ¶

Deleted: VI

Deleted: CRUDE OIL

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Deleted: within 90 days of receipt

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Deleted: and metals ( e.g. ,
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Deleted: You will need to collect at least three samples of each crude oil received by your refinery, composite these

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Deleted: Note: If you do not refine any crude oil at your facility, provide a list of the intermediate feedstocks that are refined by your facility and perform the analyses described below for those intermediate feedstocks in lieu of the crude oil composition analysis.¶

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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 collection 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 a nd 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 alternative 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 Methods 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 analysis results in Table 3. The electronic version of Table 3 is included in the electronic 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 slate that makes up the feed to the distillation column during the time of your sample is significantly different than the crude oil or intermediate slate you used during 2010

. Deleted: will be using

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Deleted: in lieu of site-specific sampling and analysis

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Deleted: and the list does not meet the definition of “equivalent” provided in Section 5 of this document,

Deleted: Crude Oil

Deleted: Total Selected Metals Concentration ... [1]

Deleted: crude oil

Deleted: separately for each

Deleted: composited samples in a Microsoft ® Excel Crude Oil Analysis Template. This Excel template

Field Code Changed

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Deleted: , click on “Petroleum Refineries”).

Deleted: identify the country

Deleted: origin and crude type ( e.g. , Texas sweet) for crude analysis. If you conducted composition analysis on more

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Deleted: , you must make a copy of the worksheet and update the crude oil type in each worksheet order to distinguish between the separate crude oil composition analyses

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### 3 You must keep the following records for 3 years:

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

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

• Description of the QA/QC procedures followed in preparing each distillation feed sample for analysis and performing the required analysis; and

• The results of the analyses performed 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 Deleted: crude oil

Deleted: crude oil

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