"CHADBOURNE John" 05/18/2007 06:01 PM To Keith Barnett/RTP/USEPA/US@EPA cc "Anderson, William" , "YBANEZ Hector" bcc Subject Essroc Sampling and Analysis - EPA request for mercury and TOC information History: This message has been forwarded. Keith, Essroc will begin sampling next Monday, May 21, 2007 to comply with the May 8 letter from Peter Tsirigotis. I have been assigned responsibility for ensuring the success of the Essroc sampling and analysis program. Hector Ybanez asked that I prepare this note to you clarifying issues that may have the potential to cause concerns. I have attached an email distributed yesterday to plant environmental engineers and quality control chemists concerning sampling requirements. Please review that document and let us know if you have a different view on any of the issues raised for sample collection. The methods referenced in Mr. Tsirigotis' letter are essentially "SW846" methods. Essroc has retained Severen Trent Laboratories (STL) to provide guidance and analytical capabilities to accomplish the sampling and analysis required. Dr. William Anderson of STL and I have discussed a number of issues raised on review of the methods to be applied to determine the mercury and Total Organic Carbon (TOC) concentration in the thousands of samples that will be taken. Dr. Anderson has pointed out that SW846 methods are guidelines to which professional judgment must be applied to produce practical, accurate results. This is explained in various chapters of SW846 where it becomes clear that the quality of the results is the responsibility of the analytical laboratories, even when difficulties arise in the application of the SW846 methods. Essroc intends to use a direct mercury analysis method that is in accord with Method 7473 and capable of detecting concentrations as low as 20 parts per billion (ppb). Depending on results, some samples will also be analyzed using HF total digestion procedures to compare results with the direct mercury analysis. The laboratory Essroc has selected will follow the quality control guidelines for duplicate, spiked and calibration samples as specified in the method. Analytical reports will include the time the samples were received and analyzed in addition to sample identification parameters. The samples will be retained on site at the analytical laboratory through at least September, 2007 so that confirmatory analyses can be provided as needed. Since the all of the samples have been exposed to ambient or high temperatures, there will be no need to refrigerate any of the samples. In addition, the usual 28 day holding time for mercury samples will not apply. No change in the mercury concentrations for these samples is expected under long-term (six month or greater) storage. Given the huge number of samples, the nature of the samples and the ability to confirm previous results with reanalysis and comparative analytical methods, the guidelines for refrigeration and holding time shall not apply. Analysis for TOC will be conducted using the Lloyd Kahn modification of Methods 9060 and 9060a. One of the laboratories selected to do these analyses employs a Shimadzu SSM-5000A TOC analyzer. We understand that phosphoric acid is substituted for hydrochloric or sulfuric acids where samples high in carbonates are to be analyzed. As explained above, no refrigeration or holding times are required to provide accurate analyses of these samples. For some materials, TOC results will be lower than the quantification limit of 500 ppm. It would be unreasonable to run hundreds of "non-detect" samples, when this information can be obtained by analyzing composite samples plus randomly selected daily samples. In order to determine which daily samples need to be analyzed for TOC, the laboratory will prepare composite samples representing two week or longer intervals from the daily composite samples. If all of the long-term composite samples and selected daily composite samples of a particular material (for example, Bessemer Kiln 1 slurry feed) are below 500 ppm, no further analyses for TOC for that material will be conducted. The TOC concentration will be reported as less than 500 ppm. For materials which demonstrate the presence of measurable levels of TOC, multiple analyses of daily composite samples will be run to determine the average and variability of TOC results. The requirement for quadruplicate analyses specified in methods 9060 and 9060a will not apply. Rather, the laboratory analyst will determine the number of additional samples to be analyzed based on the results for each sample analyzed. I feel sure you will appreciate the need to focus resources on the most important questions as we undertake this voluminous sampling and analysis program. If you have any questions or comments, please call me at 610 837 3336 or send an email. Dr. John F Chadbourne Senior Environmental Engineer Essroc Cement Corp. 3251 Bath Pike Nazareth, PA 18064 Essroc Cement Corp. CONFIDENTIALITY NOTE: This message is intended exclusively for the party or parties to whom it is addressed. This communication may contain information that is proprietary, privileged or confidential or otherwise legally exempt from disclosure. If you are not one of the named addressees, you are not authorized to read, print, retain, copy or disseminate this message or any part of it. If you have received this message in error, please notify the sender immediately by e-mail and delete/destroy all copies of the message. Any views or opinions presented in this email are solely those of the author and might not represent those of Essroc Cement Corp. WARNING: Although Essroc Cement Corp. has taken reasonable precautions to ensure no viruses are present in this e-mail, the company cannot accept responsibility for any loss or damage arising from the use of this email or attachments. Essroc Cement Corp. ----- Message from "CHADBOURNE John" on Thu, 17 May 2007 18:24:10 -0400 ----- To: "ANDREWS Mark" , "AYALA MELENDEZ Nivia" , "CAWTHRAY Mike" , "CONN Corey" , "CONSTANT David" , "DUETTA Dale" , "HARP Allen" , "HITT David" , "LUNGU Radu" , "RIVERA Beatriz" , "SHAW Derek" , "YBANEZ Hector" cc: "AYALA MELENDEZ Nivia" , "CORDER Rebecca" , "COSTELLO James" , "DUBCHAK Patricia" , "EATON Melissa" , "EMMERT Allen" , "FARMER Kelly" , "GROTHEER Kevin" , "KLEMICK William" , "LEGATE Harold" , "STOFFICK Thomas" , "WILT Larry" , "JANY Lou" , "CORDER Rebecca" , "RIZZI Fabio" , "DIDION Josh" , "Anderson, William" , "Carswell, Patti" , Subject: Sample Preparation for Shipment to Analytical Laboratories Folks, As we agreed in the conference call last Friday, the samples to be taken to comply with the EPA Section 114 letter that Essroc received last week need to be collected with rigorous quality assurance protocols. Representatives of Severen Trent Laboratories (STL) have assisted us by preparing master sample logs, daily sample collection sheets and request for analysis/chain of custody forms. All samples sent to the laboratories must be homogeneous dry powder. The laboratories will remove a sample (<1 gram) from each container. The sample you send must be a sample from which a representative aliquot can be removed with no further preparation. For samples of fuel taken from the burner pipe, CKD and ground feed to sent to the kiln, fine dry powders are collected directly at the sampling locations. For clinker samples, please grind the samples finer than ~200 mesh before preparing split samples. For slurry from wet-process kilns, please dry the samples as you normally do and retain excess dried feed material to prepare your daily composite samples. For raw material components, minimal drying is recommended, so long as a homogeneous "dry" powder is produced for sample splitting. A clay or other material with high water affinity can be dried at 105 C as necessary to produce a dry powder. Excessive drying must be avoided. Sample splitting into thirds is accomplished by thoroughly shaking the container of dry powder to achieve a homogeneous mixture. Remove approximately 200 grams of material from the thoroughly-shaken composite sample mixture and place it on a clean sheet of paper. Carefully divide the pile of dry powder into "sixths" using a clean spatula to divide the pile. Remove two "opposite" sixths into one of the sample containers to prepare the first split sample. The two remaining "opposite sixths" to prepare the second split sample. The remaining sample is placed into a third sample container. One of the samples will be analyzed for mercury, another for TOC and the third will be archived for repeat or subsequent analysis. The sample containers shipped from STL will be packaged with five cases (24 count) per shipping box. The packaging materials must be saved so that the samples can be shipped to the laboratories in the same shipping materials. This procedure will minimize breakage. Collect mercury samples in one set of sample cases until 5 cases have been accumulated. A plant collecting 10 mercury samples per day will fill the sample shipping box in 12 days of sampling. (10 samples per day X 12 days of sampling = 120 samples = 5 cases X 24 samples per case). There is no need to refrigerate samples. The materials used to manufacture cement are stored at ambient temperatures and exposed to high temperatures in the pyroprocess. Mercury present in feed to the raw mills will be stable as complex mercury minerals. Since the only constituents to be measured are mercury and TOC, you may use grinding equipment which contains chromium metal to prepare these samples. The amount of chromium contamination possible from chromium grinding equipment in this instance is acceptably low. Please complete the daily sample collection log that describes the time when each component of the composite sample was collected. The initials of the individual should be entered in addition to the time when the sample was collected. At least three samples are needed for each daily composite sample, unless an equipment failure prevents collection of a "shift" sample. In the case where equipment outages result in a "short sample" it is best to start preparation of another complete composite sample. If a "short" composite sample is submitted for analysis, it is essential that notes on the sample collection sheet describe the reason for collecting that sample. When a shipment of samples has been collected, split and packaged for delivery to the laboratories, a request for Analysis/Chain of Custody sheet will need to be prepared and sent with the samples. All mercury analyses for the first round of samples will be completed by: G & C Coal Analysis Lab., Inc. Attn: Michael J. Chestnut 1341 Hoffman Hollow Rd Summerville, PA 15864 (814) 849-7301. Information on TOC analysis will be distributed soon. Please call me or send email if there are any questions or concerns. John Essroc Cement Corp. CONFIDENTIALITY NOTE: This message is intended exclusively for the party or parties to whom it is addressed. This communication may contain information that is proprietary, privileged or confidential or otherwise legally exempt from disclosure. If you are not one of the named addressees, you are not authorized to read, print, retain, copy or disseminate this message or any part of it. If you have received this message in error, please notify the sender immediately by e-mail and delete/destroy all copies of the message. Any views or opinions presented in this email are solely those of the author and might not represent those of Essroc Cement Corp. WARNING: Although Essroc Cement Corp. has taken reasonable precautions to ensure no viruses are present in this e-mail, the company cannot accept responsibility for any loss or damage arising from the use of this email or attachments. Essroc Cement Corp.