### FW: Laboratory method for NMP Gary Wood to: Christopher Lambesis Cc: "Jeff Glaser" 06/04/2010 03:35 PM

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History: "Gary Wood" <woodgl@trimatrixlabs.com >

Christopher Lambesis/R5/USEPA/US@EPA "Jeff Glaser" <glaserj@trimatrixlabs.com > Please respond to <woodgl©trimatrixlabs .com> This message has been replied to.

Hi Chris,

I pulled the email Terri Zick had sent me regarding how we were going to proceed with this program. Below her message is yours saying to include a raw product sample for the purposes of identification. At that point, at least, we hadn't discussed using it for a 1pt calibration.

Our Lab Manager has reviewed the data and sent me a response to your concern about our IS's failing and/or our analytical system not being in control. I've copied the text of his message into this email. It is as follows:

Gary - I took a look at the data for this and there were some issues with the samples, but nothing was wrong with the instrument. Several of the samples had internal standards recoveries that were outside of the method acceptance windows, however, the analyte we were looking for, N-methylpyrrolidone, is associated with the internal standard 1,4-dichloorobenzene-d4, which was in control in all of the samples. All of the samples also had out of control acid surrogate recoveries, and one had a base-neutral surrogate that was out of control (1003151-05). The analyte of interest is not an acid compound, so the only sample that might be considered as suspect would be 1003151-05. However, from reviewing the chromatograms, the reason for the low recoveries was matrix interference from high concentrations of other "non-target" analytes. We could have gone and diluted the sample and reanalyzed them, but all that would have done was elevate the reporting limits and all samples would have been non-detect; there wouldn't have been any useful data at all in that case. I think that we need to keep in mind that we are talking about estimated concentrations for these anyway, so the surrogate recoveries and non-associated internals really lose their relevance. Please let me know if you have any other questions.

Jeff P. Glaser Vice President, Laboratory Operations

As always Chris, let me know if you have questions orwoodgl@trimatrixlabs can do to help.

Thank you,

Gary Wood Senior Project ChemistCorporate / Laboratory

616.975.4500 5560 Corporate Exchange Court SE Grand Rapids, Michigan 49512 woodgl@trimatrixlabs.com Main:

Direct: 616.940.4206
Fax: 616.942.7463 www.trimatrixlabs.com

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Original Message From: Terri Zick [mailto:tzick@cticompanies.com] Sent: Wednesday, March 03, 2010 11:53 AM To: woodgl@trimatrixlabs.com ; glaserj@trimatrixlabs.com ; roudbushw@trimatrixlabs.com Cc: Mike Movinski Subject: FW: Laboratory method for NMP

GentlemenThe EPA folks have indicated that they will accept results from samples run for NMP as a TIC. They are also looking to have us run a diluted sample of the raw product as a comparison (see e-mail below). I look to your expertise to clarify for me what we need to consider to obtain defensible data from this effort and to put a price-tag on the effort. We will need to collect the samples before 3/11/10, so I would like to make sure we have bottles in the next couple of days and have a general idea of approach and cost. I do not want to blind-side my client with costs that they do not expect.

Thank you for your technical expertise and help!!!

Terri Zick 313-300-7401 cell tzick@cticompanies.com

CTI and Associates, Inc. 51331 W. Pontiac Trail, Wixom, MI 48393 248.486.5100 Phone I 248.486.5050 Fax

Original Message From: Lambesis.Christopher@epamail.epa.gov [mailto:Lambesis.Christopher@epamail.epa.gov] Sent: Wednesday, March 03, 2010 11:09 AM To: Terri Zick Cc: Kathy Wilson; Ramaly.Todd@epamail.epa.gov Subject: Re: Laboratory method for NMPTerri,

We agree to your proposed sampling and analysis methods for NMP as suggested below. I also suggest you separately send for analysis a sample of the raw NMP product (about 10m1 in a VOA vial). It is important that the laboratory is notified that this sample is pure product and should be diluted accordingly. Analysis of the diluted NMP product should help identify chromatographic retention time and possible breakdown constituents without derivatization.

Christopher Lambesis Environmental Scientist U.S EPA Region 5 Land and Chemicals Division (312) 886-3583

From: Terri Zick <tzick@cticompanies.com >

To: Todd Ramaly/R5/USEPA/US@EPA, Christopher Lambesis/R5/USEPA/US@EPA

Cc: Kathy Wilson <kathywilson@owossographic.com >

Date: 03/02/2010 12:35 PM

Subject: Laboratory method for NMP

We have confirmed with Trimatrix Laboratories that Method 8270 will be the appropriate method under which to look for NMP as a TIC (Please see the pertinent excerpt from their e-mail response below)

We propose collecting 3 composite samples from the roll-off box which is currently full & scheduled for shipment on March 11, 2010. The filter cake in the box represents 6 press cleanings within the past 75 days. We propose collecting a series of 3 samples, each composited from 2 locations within the container. Two samples would be collected from the north third, 2 from the central portion of the box and 2 from the south end of the box. Each set of 2 samples would be composited to constitute a single sample and analyzed using method 8270 without a method 1311 extraction. The chromatograms from the analysis will be used to identify NMP, if present, as a TIC.

While TIC's are, by definition, not validated results in the same way that a sample is validated against a standard, the method blank, surrogate and internal standard recovery, and the DFTPP tune summary will demonstrate that the sample was run on an analytical system that was in control and valid for the method by which the sample was analyzed. If the laboratory detects hits of this compound in these samples, the raw data will include the library search report along with the supporting data we used to make the tentative identification so a 3 rd party reviewer could confirm those results using information from the data package.

Based on production, Owosso Graphic Arts is shipping every 90 or fewer daysso the window of opportunity for sample collection is small. We would like

to come to concurrence on the number of samples that you would deem acceptable and confirmation that you find the analytical approach using method 8270 appropriate for your purposes.

Thank you in advance for your review & response.

Terri Zick 313-300-7401

Hi Terri,

I had our Lab Manager review this. Method 8270 would be our best bet. We have no standard for it, so it would have to be done as a TIC.

Gary Wood Senior Project Chemist

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Corporate Laboratory Main: 616.975.4500 5560 Corporate Exchange Court SE Direct: 616.940.4206 Grand Rapids, Michigan 49512 Fax: 616.942.7463 woodgl@trimatrixlabs.com www.trimatrixlabs.com

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