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What procedures should independent labs use to identify the samples for analysis under the 10% independent analysis option? What samples will EPA want to receive from independent labs?

Please see the following Protocol. (10/3/94)

REFORMULATED GASOLINE PROGRAM

INDEPENDENT SAMPLING AND TESTING REQUIREMENTS

PROTOCOL

FOR USE BY INDEPENDENT LABS IN SELECTING SAMPLES FOR ANALYSIS UNDER THE 10% INDEPENDENT ANALYSIS OPTION, AND FOR IDENTIFYING SAMPLES TO SHIP TO EPA.

1.0 General Instructions.

1.1 This protocol constitutes EPA identification under § 80.65(f)(1)(ii)(B) of samples that must be analyzed for refiners and importers using the 10% independent analysis option of § 80.65(f)(1)(ii), and must be followed separately for each refinery or importer for which the independent lab is being used to fulfill the 10% independent analysis option. This protocol also constitutes EPA identification under § 80.65(f)(3)(iv) of samples that independent labs must ship to EPA .

1.2 In the case of the 10% independent analysis option, this protocol must be used to select the samples for analysis for each two week period. Each two-week period begins on Sunday night at midnight, and lasts for the subsequent two weeks. The first two-week period begins at midnight on August 7, 1994, the second two-week period begins at midnight on August 21, 1994, etc.

1.3 This protocol may be replaced at any time by EPA with different instructions for selecting samples for analysis under the 10% independent analysis option, or for shipping samples to EPA.

1.4 EPA may issue special instructions for selecting samples for analysis or shipping to EPA for any specific refiner, refinery, importer, or independent lab that differ in whole or in part from the instructions contained in this protocol, and if such special instructions are issued they must be followed instead of the instructions contained in this protocol.

1.5 Definitions:

RFG - reformulated gasoline

RBOB - reformulated gasoline blendstock for oxygenate blending

2.0 Identify Samples for the Current Analysis Cycle.

2.1 Identify each sample of RFG or RBOB collected during the preceding two-week period, and the refiner or importer assigned batch identification number for each sample.

2.2 Add any samples carried over from a prior analysis cycle, from 3.2 and 3.4.1.

2.3 Order the samples from the preceding two-week period, plus any carry over samples, in chronological order using the batch identification number for each sample.

3.0 Determine the Number of Samples to be Analyzed.

3.1 The number of samples that must be analyzed for the current analysis cycle is the number of samples identified under step 2.0 that is evenly divisible by ten.

3.2 Any remainder from this division is the number of samples that must be carried over to the subsequent analysis cycle. Any carry over samples must be those with the largest batch identification numbers.

For example, if the number of samples identified under step 2.0 is thirty seven, with batch numbers 4321-54321-95-002534 through 4321-54321-95-002570, the number of samples that must be analyzed in the current analysis cycle is three, and seven samples must be carried over to the subsequent analysis cycle. The specific samples that must be carried over are those seven with the largest batch identification numbers, or samples 4321-54321-95-002564 through 4321-54321-95-002570.

3.3 To the extent any sample carry over would result in a sample being retained by the independent lab for more than 30 days, this protocol constitutes EPA's request under § 80.65(f)(3)(ii) to retain the sample for more than 30 days. This additional sample retention request is for the length of time until the sample is not carried over to a subsequent analysis cycle, but for a maximum of 180 days.

3.4 Case Where Number of Samples is Less than Ten

3.4.1 If the number of samples identified under step 2.0 is less than ten, then all samples should be carried over to the subsequent analysis cycle.

3.4.2 If, however, the number of samples identified under step 2.0 is less than ten, and any sample carry over would result in a sample being retained for more than 180 days, then one sample must be analyzed from the number, and none of the samples would be carried over to the subsequent analysis cycle.

4.0 Identify Which Samples to Analyze

4.1Identify the beginning point for using the Random Number Table at 4.2 for the current analysis cycle.

4.1.1 Identify the last two digits from the closing point for the Dow Jones Industrial Average as reported in the Wall Street Journal for the first day the New York Stock Exchange is open following the close of the preceding two-week period.

For example, for the two-week period ending at midnight on Sunday, August 20, the relevant two digits would be the last two digits for the close for the Dow Jones Industrial Average for Monday, August 21, as reported in the Wall Street Journal for Tuesday, August 22. If this Dow Jones Industrial Average close is 3,741.06, the relevant two digits would be 06.

4.1.2 The beginning point for the Random Number Table at 4.2 for the current analysis cycle is the row number (from Column A of Table 4.2) that corresponds to the number identified under

4.1.1.

Using the example from 4.1.1, the applicable row number would be 06, and the first random number would be 27.

4.2 Random Number Table

Column
A B

Column
A B

Column
A B

 00 60  39 91  78 65
 01 77  40 95  79 29
 02 38  41 01  80 64
 03 16  42 02  81 57
 04 45  43 76  82 59
 05 39  44 79  83 83
 06 27  45 19  84 10
 07 93  46 11  85 52
 08 97  47 88  86 53
 09 37  48 73  87 30
 10 06  49 43  88 48
 11 18  50 74  89 69
 12 98  51 12  90 24
 13 05  52 31  91 62
 14 92  53 85  92 99
 15 72  54 94  93 51
 16 71  55 35  94 56
 17 87  56 40  95 36
 18 20  57 55  96 08
 19 41  58 86  97 14
 20 00  59 34  98 07
 21 78  60 22  99 44
 22 33  61 46  
 23 61  62 89  
 24 75  63 70  
 25 25  64 50  
 26 54  65 03  
 27 80  66 09  
 28 32  67 67  
 29 17  68 42  
 30 15  69 82  
 31 63  70 84  
 32 04  71 96  
 33 21  72 28  
 34 90  73 66  
 35 68  74 49  
 36 58  75 23  
 37 13  76 26  
 38 47  77 81  

4.3 For each sample for the current analysis cycle under 2.0, excluding any samples carried over to the subsequent analysis cycle under 3.2 or 3.4.1, identify the last two digits of the batch identification number.

This process is illustrated in the following table:

If the batch number is: The last two digits are:

4321-54321-95-002533 334321-54321-95-002593 93

4.4 Compare the two digit number from Column B of the Random Number Table at the beginning point identified under 4.1.2 (the first random number) with each of the two digit sample numbers Identified under 4.3.

4.5 If the first random number matches any sample number, this sample is identified as a sample for analysis. If the random number matches more than one sample number, only the sample with the lowest batch identification number is identified as a sample for analysis.

4.6 If the first random number does not match any sample number, then move to the next number in the Random Number Table, and repeat the process described under 4.5.

In the example under 4.3, there is no match for the first random number (27), but there is a match for the second random number (93), and sample number 4321-54321-95-002593 would be identified for analysis.

4.7 Continue this process until the number of samples identified for analysis equals the number under 3.1 or 3.4.2.

5.0 Analysis of Identified Samples

5.1 Proceed to analyze each sample identified under 4.0 as specified under § 80.65(f)(1)(ii)(C).

5.2 If a sample to be analyzed is of RBOB, the sample first must be blended with the applicable amount and type of oxygenate. The following chart specifies this oxygenate blending with RBOB:

 RBOB Type  Oxygenate Type  Oxygen Volume
 Any-Oxygenate  Ethanol 2.0 wt%
Ether-Only MTBE 2.0 wt%
Any-Renewable-Oxygenate Ethanol 2.0 wt%
Renewable-Ether-Only ETBE 2.0 wt%
Non-VOC-Controlled-Renewable-Ether-Only ETBE 2.0 wt%
Refiner-Specified 13 14

This requirement to blend RBOB with oxygenate applies to refiners and importers who are using both the 10% independent analysis option under § 80.65(f)(1)(ii) and the 100% independent analysis option under § 80.65(f)(1)(i).

6.0 Shipment of Samples to EPA

6.1 Quality Assurance Samples

For purposes of quality assurance oversight, a portion of certain samples must be sent to EPA, under § 80.65(f)(3)(iv), at the frequencies specified in this item 6.1. This requirement applies to refiners and importers who are using both the 10% independent analysis option under § 80.65(f)(1)(ii) and the 100% independent analysis option under § 80.65(f)(1)(i). EPA may specify a different frequency for sending quality assurance samples to EPA for any refiner, refinery, importer, or independent lab, and if such different frequency is specified it must be followed.

6.1.1 Refiners and Importers Using the 10% Independent Analysis Option

6.1.1.1 In the case of samples identified for analysis under 4.0, for each thirty-third sample that is analyzed for each refinery or importer a portion of the sample must be sent to EPA.

6.1.1.2 In the case of samples that are not identified for analysis under 4.0, each thirty-third sample that is collected for each refinery or importer but that is not analyzed by the independent lab must be sent to EPA.

6.1.2 Refiners and Importers Using the 100% Independent Analysis Option

For every thirty-third sample that is analyzed for each refinery or importer, a portion of the sample must be sent to EPA.

6.2 Samples That Violate Applicable Standards

6.2.1 In the case of refiners or importers who are using the 100% independent analysis option, a portion of each sample that violates an applicable per-gallon standard must be sent to EPA.

6.2.2 The applicable standards are those specified under § 80.41. In the case of parameters being met on a per-gallon basis, the per-gallon standards are the applicable standards. In the case of parameters being met on an average basis, the per-gallon minimums and maximums are the applicable standards.

6.3 Shipping of Samples

6.3.1 Each sample sent to EPA must be sealed in containers and transported in accordance with the procedures specified in Appendix D to 40 CFR Part 80, and identified with the independent lab's name and registration number and the sample information specified in § 80.65(f)(3)(i).

6.3.2 The quantity of sample that must be sent is: in the case of samples that have been analyzed by the independent lab, the entire volume remaining following the laboratory analysis which should be a minimum of one pint; and in the case of samples that have not been analyzed by the independent lab, the entire volume that is collected by the independent lab, or a minimum of one quart.

6.3.3 Samples identified for shipping to EPA under 6.1 or 6.2 must be sent to EPA via an overnight package service to:

United States Environmental Protection AgencyMotor Vehicle and Fuels Emissions LaboratoryFuels and Chemicals Analysis Branch2565 Plymouth RoadAnn Arbor, Michigan 48105

(313) 668-4200

13 The oxygenate specified in the refiner's instructions, or if more than one oxygenate is allowed, from the following list of oxygenates the first that is allowed by the refiner's instructions: ethanol, MTBE, ETBE, any other specified oxygenate.
14 The volume specified in the refiner's instructions, or if a range is specified, the minimum vol% oxygenate allowed.

This question and answer was posted at Consolidated List of Reformulated Gasoline and Anti-Dumping Questions and Answers: July 1, 1994 through November 10, 1997 (PDF)(333 pp, 18.17 MB, EPA420-R-03-009, July 2003, About PDF)