Document ID: EPA-HQ-OW-2010-0192-0216
Agency: epa
Document Type: Supporting & Related Material
Title: 
Posted Date: 2011-12-14T05:00Z

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.