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PART VII. SUMMARY OF TEST PROCEDURES, METHODS, AND 

REPORTING REQUIREMENTS FOR DISTILLATION FEED COMPOSITION 

ANALYSIS 

The EPA petroleum refinery test program 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 distillation 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 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 distillation 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

Deleted: crude oil-based HAP.

Deleted: crude oil composition 

Deleted: .

Deleted: within 90 days of receipt

Deleted: crude oil

Deleted: and metals (e.g., 

Deleted: ).

Deleted: You will need to collect at least three 

samples of each crude oil received by your refinery, 

composite these

Deleted: crude oil

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.¶

Deleted: crude oil
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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 and 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/ft3

 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 

Deleted: analysis from a

Deleted: in lieu of site-specific sampling and 

analysis

Deleted: crude oil

Deleted: crude oil

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

Deleted: http://icr2010

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

Deleted: one type of

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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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 Results

Sample Date

Unit ID for Distillation Column

Higher Heating Value (Btu/lb)

Density (lb/ft3

)

API Gravity

Concentrations (ppm)

Unit IDs for Other Distillation 

Column(s) with Feed 

Representative 

If the crude oil or intermediate slate 

being fed to the distillation column 

during the time of this sample is 

significantly different than the 

crude oil or intermediate slate used 

during 2010, briefly explain

Mercury

Chlorine

Sulfur

Antimony

Arsenic

BerylliumCadmium

Chromium

Cobalt

Lead

Manganese

Nickel

Selenium

Deleted: crude oil

Deleted: crude oil

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