Component 3 Form Approved 03/28/2011 

OMB Control No. 2060-0657 

Approval Expires 03/31/2014 

1 

Petroleum Refinery 

Emissions Information Collection 

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 and analyze samples of the feed to your distillation column(s) 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 to collect the first sample during April, the second during May, and the third during 

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. 

For the purposes of this request, you may elect either to sample the crude oil (or other petroleum 

stream first processed) from the storage tank that supplies the distillation column or to take 

samples from the line feeding the distillation column. For atmospheric crude distillation units 

with desalters, you may elect to sample either before or after the desalter; you must indicate 

where the sample was taken. 

If you have multiple distillation columns and the feed to each is similar, you must collect 

samples from each distillation column and composite them so that only one sample is analyzed 

per month. If you have multiple distillation columns that receive intentionally different feed 

streams, then you must collect and analyze separate samples for each distillation column 

receiving different feed streams. For example, if you have three distillation columns and two 

have the same feed, you would collect samples from the first two and composite those into one 

sample to analyze each month, and you would also collect samples from the third distillation 

column and analyze those samples separately. 

 

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). 
Component 3 Form Approved 03/28/2011 

OMB Control No. 2060-0657 

Approval Expires 03/31/2014 

2 

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

should be collected. When sampling from storage tanks, remove a minimum of three 

discrete, equal-volume grab samples from different locations in the tank and composite 

these samples for subsequent analysis. If you collect samples from the feed line, you 

must collect a minimum of three equal-volume samples with a minimum of 5 minutes 

between samples; these samples should then be composited for subsequent analysis. If 

you have multiple distillation columns with similar feed, collect an equal number of 

equal-volume feed samples from each distillation column and composite all of the 

samples for analysis. In other words, if there are two distillation columns with similar 

feed, collect a minimum of two equal-volume samples from each distillation column to 

prepare the composite. If there are three or more distillation columns with similar feed, 

collect a minimum of one equal-volume sample from each distillation column to prepare 

the composite. 

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. 
Component 3 Form Approved 03/28/2011 

OMB Control No. 2060-0657 

Approval Expires 03/31/2014 

3 

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. 

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. 
Component 3 Form Approved 03/28/2011 

OMB Control No. 2060-0657 

Approval Expires 03/31/2014 

4 

Table 3. Distillation Feed Sample and Analysis Results 

Unit ID for One Distillation Column with Feed 

in the Composite Sample1

Unit IDs for Other Distillation Column(s) with 

Feed in the Composite Sample1

Sample Date 

Indicate if the sample was collected before or 

after the desalter (Before/After/Not Applicable) 

Higher Heating Value (Btu/lb) 

Density (lb/ft3) 

API Gravity 

Concentrations (ppm) 

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, 

Mercury 

briefly explain 

Chlorine 

Sulfur 

Antimony 

Arsenic 

Beryllium Cadmium 

Chromium 

Cobalt 

Lead 

Manganese 

Nickel 

Selenium 

 

 

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 Enter the Unit ID provided in Component 1. If the composite samples include feed from more than one distillation column, 

enter the Unit ID for one distillation column in the first column of the table and the Unit ID for the other distillation column in 

the second column of the table. If the composite samples include feed from more than two distillation columns, enter the Unit 

ID for one distillation column in the first column of the table and the Unit IDs for the other distillation columns in the second 

column of the table.