ASTM D19.06 SUBCOMMITTEE

STUDY PLAN FOR THE TESTING OF ADDITIONAL INDUSTRIAL

WASTEWATER MATRICES IN SUPPORT OF ASTM STANDARD D7575

FOR USEPA’s RECONSIDERATION OF THIS METHOD IN THE

FORTHCOMING METHOD UPDATE RULE

Prepared for:

United States Environmental Protection Agency

Office of Water

Engineering and Analytical Support Branch

September, 2011
INTRODUCTION

This document is in response to the United States Environmental Protection Agency

(EPA) Office of Water, Engineering and Analytical Support Branch request to conduct and

provide test results from additional industrial water matrices in support of its reconsideration of

ASTM Standard D7575 (Standard Test Method for Solvent-Free Membrane Recoverable Oil and

Grease by Infrared Determination) for inclusion in EPA’s forthcoming Method Update Rule

(MUR).

The remainder of this document provides the details of the draft study plan for

conducting the additional testing.

STUDY NAME

The name of this study is: “Testing of Additional Industrial Wastewater Matrices in

Support of USEPA Reconsideration of ASTM Standard D7575 in the Forthcoming Method

Update Rule.”

STUDY DIRECTION AND SPONSOR

This study is under the direction of ASTM D 19 Water. The study is being sponsored

and managed voluntarily by the technical members of the ASTM D19.06 Sub-committee for

ASTM Standard D7575.

STUDY DESIGN

Summary

The design of this study will be similar to those in the previous single-laboratory studies

used for standardization of ASTM D7575. In summary, wastewater from applicable industries

acceptable to the study objectives will be collected according to standard EPA protocols and

shipped to the OSS laboratory for initial screening of oil and grease by ASTM Standard D7575

to ensure the concentration within the sample is within the range of the method. The industrial

matrices that pass this screening will then be sent to a designated laboratory for oil and grease

determination by EPA Method 1664 and ASTM Standard D7575. Upon completion of sample

analyses, ASTM D19.06 sub-committee will review the results and prepare a written study

report, which will then be submitted to EPA’s Engineering and Analytical Support Branch.

Sample Matrices

A minimum of three industrial matrices will be collected and evaluated for this study.

The sample collection process will follow the sampling procedures of EPA’s Freon replacement

studies during the development of EPA 1664, whereby one large single grab is collected and

sample bottles are split from that original grab while being mixed. The minimum three matrices
will be of the following categories (examples of the types of matrices that are being sought are

given):

• Petroleum Refining and Related Industries – SIC 29 (e.g. refinery facility that processes

raw crude oil into multiple petroleum products including petroleum grease-related

products)

• Food and Kindred Products Manufacturers – SIC 20 (e.g. meat processing facility that

performs a full spectrum of animal processing including slaughtering, meat product

manufacturing, and rendering beef and/or pork )

• Chemicals and Allied Products – SIC 28 (e.g. chemical manufacturer that falls within

EPA’s regulation category of organic chemicals, plastics, and synthetic fibers (OCPSF) )

The goal of sample collection of these matrices will be to ensure that the total oil and grease

concentrations are within the ASTM D7575 operating range (5ppm – 200ppm).

Study Methods

The two methods used for this study will be EPA Reference Method 1664 (hexane

liquid/liquid extraction) and ASTM Standard D7575.

Study Laboratories

The laboratories identified for this study will include OSS for initial screening of

matrices to ensure that they are within the operating range of D7575 and a centralized

commercial laboratory using EPA Method 1664 and ASTM D7575 for oil and grease on the

same collected industrial matrix samples.

Standardized Quality Control Tests

Under this study, the following standardized quality control (QC) tests will be performed

with each matrix, for each of the two methods:

• Field matrix sample in triplicate

• Field matrix sample spike (hexadecane and stearic acid per EPA Method 1664 protocol)

• Field matrix sample spike duplicate (hexadecane and stearic acid per EPA Method 1664

protocol)

• Reagent blank

• Laboratory Control Spike

• Laboratory Control Spike Duplicate
Statistical Analysis

Precision of Triplicate Field Sample Analyses – Triplicate analyses of each matrix will be

tested for precision by calculating the percent relative standard deviation (standard deviation

divided by the mean concentration X 100).

Accuracy and Precision of Matrix Spike and Matrix Spike Duplicate Analyses - The matrix

spike and matrix spike duplicate (MS/MSD) test is used to assess method performance in the

sample matrix. Analytes of interest (hexadecane and stearic acid) are added to a field sample

aliquot that is then thoroughly homogenized and split into two spiked replicate aliquots for

analysis. One of these replicates is identified as the matrix spike sample and the other is

identified as the matrix spike duplicate sample. The recovery of the analytes relative to the spike

concentration is determined in each sample. Accuracy is measured from the difference in

determination of the spiked sample and unspiked field sample divided by the spiked amount,

multiplied by 100. The precision of the determinations is assessed by measuring the relative

standard deviation of recovery.

Accuracy and Precision of Laboratory Control Spike and Laboratory Control Spike

Duplicate - The laboratory control spike and laboratory control spike duplicate (LCS/LCSD) test

is used to assess method performance in a controlled reference matrix. Analytes of interest

(hexadecane and stearic acid) are added to reagent water that is then thoroughly homogenized

and split into two spiked replicate aliquots for analysis. One of these replicates is identified as

the laboratory control spike sample and the other is identified as the laboratory control spike

duplicate sample. The recovery of the analytes relative to the spike, are determined in each

sample. Accuracy is determined from the average of the two recoveries of spiked samples

divided by the spiked amount, multiplied by 100. The precision of the determinations is assessed

by measuring the relative standard deviation of recovery.

Study Report

Upon final review of the sample analyses, the ASTM D19.06 subcommittee will draft a

report of the study findings. Once approved by the ASTM D19.06 Sub-committee, the report

and raw data will be sent to the EPA’s Engineering and Analytical Support Branch.

Study Timeline

The goal is to complete this study by November 15, 2011.