Document 8V6Ex0YpbY36rd60V25VbpBDe

AR226-2571 To: Andrew S Hartten/AE/DuPont@DuPont cc: Subject: Protocol for sampling and testing Forwarded by Isidores J Zan ikos/A E /D u Pon t on 10/02/2001 02:55 P M $ George H Senkler_Jr ' 10/02/2001 01:32 PM To: Isidores J Zanikos/AE/DuPont@DuPont, Mary A Kaiser/AE/DuPont@DuPont cc: John R Bowman/A/DuPont@DuPont Subject: Protocol for sampling and testing Per our discussion of last week, l have taken the materials that Mary had provided and crafted a document that might provide the "road map" for the procedures we use to map, sample and test, I would very much approcuiate your comments as to the adequacy of these instructions. W hen I have incorporated your comments, I will send In it to John for his purposes. .. ....... . ............... .. Forwarded by Isidores J Z an ikos/AE/D u Pon t on 10/02/2001 02:55 P M ----------------------- --------------- $ George H Senkler Jr ` 10/02/2001 01:35 PM To: Isidores J Zanikos/AE/DuPont@DuPont, Mary A Kalser/AE/DuPont@DuPont cc: John R Bowman/AE/DuPont@DuPont Subject: Document Sorry. Here Is the document. Water Sampling & Testing.** IID 3 1 7 1 3 4 Under Section V of the proposed Consent Order, DuPont proposes the following well survey, sampling, and testing protocols be followed. We believe that this proposal identifies third-party contractors with experience in C8 chemistry that have both the reputation for consistently delivering credible performance, and who can deliver this performance with independence of action. W ELL SURVEYING We believe that it would be useful to employ a contractor with experience in the Washington Works area to do the well survey work call For in Section V, Subsections A and B. Our first choice for such a contractor would be Potesta Associates who was knowledge of and experience with the area in question, SAMPLING For the required sampling, we propose using Battelle Duxbuiy Operations, 397 Washington Street, Duxbury, MA 02332, Battelle has experience in conducting environmental sampling for C8 using the protocol shown below (which we would proposed is suitable for the sampling under this Consent Order): Standard Operating Procedure for collection and handling of water samples. 1.0 Objective The purpose of this standard operating procedure (SOP) is to describe the procedures that will be used to collect, store, and ship water samples collected for the project. This SOP describes sample collection methods for three types of water sources: drinking water supplies, publicly-owned treatment plants (POTW), and land fills, 2.0 Preparation 2.1 Supplies and Equipment Polyethylene ja r - 1 Liter, pre-deaned, certified Polyethylene ja r - 250 g, pre-cleaned, certified Stainless steef scoop or spoon G am in 12% hand-held GPS HPLC-grade Methanol Chem wipes Ice Cooler Safety glasses Nitrile gloves Zip-sealed bags (sealed immediately upon purchase) 2.2 Applicable Documents Project Survey Plan (to be supplied to the sampling contractor) Labels Cham-of-custody forms Letters o f permission (as needed) 2.3 Decomtamination Procedures Any sampling equipment that is re-used must be thorough cleaned between each sample. To clean the sampling equipment: Wipe off any residual sludge or water with a Chem wipe. Rinse the equipment with deionized water. Rinse the equipment with methanol. Place in zip-sealed bag until next use. 2.4 Sampling Locations Water samples will be collected per the sampling plan, and will use (lie following protcol: E ID 317135 Drinking water samples will be collected at a source or sutwlv, at the drinking water facility intake, after treatment at the drinking water facility outflow, and at the point of public consumption (tap). Landfill leachate samples will be collected at well points. Publicly-owned treatment plant water samples will be collected as post-chlorination influent and effluent. If the source of municipal drinking water is ground water then any open water supply is acceptable. If a valve withdrawal system is available then follow the sampling procedures. The intake water samples should represent drinking water from the source location just prior to treatment. Thus the drinking water plant influent sampling location must be within the facility itself. Drinking Water Facility Outflow. The outflow sampling location should provide treated water that has not been exposed to "outside" air. Thus the drinking water plant outflow sampling location must be within the facility itself. Tap water will be collected at three retail establishments in the same city in which the drinking water facility is located. It is important that the water sample be untreated, therefore samples from rest rooms or outside faucets rattier than drinking fountains are required. 2.5 General Instructions Water sample bottles will not be pre-rinsed with site water prior to sample collection. The number and type of field and quality control samples to be collected are defined in the sampling plan. It is extremely important that this document be referenced prior to any sampling activity. Gloves should be worn during sampling activities and replaced between samples. All samples will be held chilled (-4 0 Q from collection to shipping. Sampling Protocol - Open Water Wipe the exterior of the sampling bottle with methanol. Submerge the sample bottle below the water surface and unscrew the bottle cap. Fill the water bottle by turning the bottle parallel to the water surface and slowing rotating so that the mouth of the bottle is up-right. This procedure will ensure that water from the surface microlayer is not pulled into the sample bottle. Recap the sample bottle under water. Wipe the bottle with methanol and affix a sample label. , Place the sample in a cooler of ice. Complete the chain-of-custody form. Sampling Protocol - valve system (faucet) Locate an appropriate tap water source. Wipe the tap water faucet and the exterior of the sampling bottle with methanol. Open tlie valve and allow water to run for at least two minutes to flush the valve system and supply lines. Remove the bottle cap, wipe the bottle lip with methanol, place the bottle under the tap, and fill. If the botttle will not fit under the tap faucet then look for another appropriate source. Do not use a secondary container to fill the bottle. Recap the sample bottle. Wipe the bottle with methanol and affix a sample label. Place the sample in a cooler of ice. Complete the chain-of custody form. E ID 317136 3.0 Qualify Control The quality control (QC) samples collected for this project are related to the type of water sample being collected. General sample collection instructions are provided below. Field Replicates will allow the analysts to measure the variability of results between two "identical" samples. Field replicates should be collected and handled exactly like the authentic field sample. A Field Replicate should be obtained with ever six (6) actual field samples taken as per the sampling plan. Field Blanks will allow the analysts to assess contamination introduced by the sampling conditions. Field blanks will be empty sample containers that are handled as if they were filled with a sample but are actually left capped throughout the sampling process and are not filled with sample. TESTING All testing will be done at an independent contractor using the liquid duomatography/tandem mass spectrometry (LC/MS/MS) method. It is strongly recommended that Exygen Research be selected as the preferred analytical laboratory because o f their prior experience in handling such samples. The method of testing should be as follows: 1. Sample Preparation for LC/MS/MS Analysis Water samples should be initially' treated with 200 gliter o f 250 mg/liter sodium thiosulfate solution to remove residual chlorine. Solid phase extraction (SPE) should then be used to prepare the samples for LC/MS/MS analysis. A forty milliliter portion o f sample should be transferred to a C|g SPE cartridge. The cartridge should then be eluted with 40% methanohwater. The eluate should be discarded. The cartridge should then be eluted with 100% methanol. A 5 milliliter portion of the methanol eluate should be collected for analysis by LC/MS/MS. This treatment results in an eight-fold concentration of the sample prior to analysis. 2. Sample Analysis by LC/MS/MS An aliquot of the extract (prepared above) is injected into the high-pressure liquid chromatograph (HPLC) and passed through a liquid-phase chromatographic column. Based on the affinity of the analyte for the stationaiy phase in the column relative to the liquid mobile phase, the analyte is retained for a characteristic amount of time. Following HPLC separation, electrospray mass spectroscopy provides a rapid and accurate means for analyzing C8. Electrospray is generally operated at relatively mild temperatures; molecules are ionized, fragmented, and detected. Ions characteristic of C8 are observed and quantitated against known standards. A Hewlett-Packard HP! 100 HPLC system coupled to a Micromass Ultima MS/MS, or equipment that is comparable in function and accuracy, is appropriate for use in analyzing the sample extracts. 3. Analysis Protocol . 3.1 Calibration: a seven-point calibration curve should be run at the beginning o f any analytical sequence and throughout the run for C8. The calibration points should be prepared at 0, 25,50, 100,250,500, and 1000 ng/liter (ppt). The instrument response versus concentration should be plotted for each point. Using linear regression with 1/x weighting, the slope, y-imercept and correlation coefficient (r) and coefficient of determination ( r ) should be determined. An acceptable calibration curve should have r greater than or equal to 0.985 (r2greater than or equal to 0.970). Calibration standards for MS/MS analysis should be prepared using the same SPE procedure used for the samples. 3.2 Blanks: Extraction blanks should be prepared and analyzed with every extraction batch of samples. The extraction blanks should not have any target analyte present at or above the concentration of the low-level calibration standard. Instrument blanks in the form of pure methanol solvent should also be analyzed after every high-level calibration standard, and after any know high-level samples. Again, the blanks should not have any target analyte present at or above the low-level calibration standard. 3.3 Duplicates: All field samples should be analyzed in duplicate. EID317137 EXD317138