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Measuring and Removing Dissolved Metals from Stormwater in Highly Urbanized Areas (2014)

Chapter: Appendix B - Detailed Cleaning Protocol for Equipment to be Used for Collection of Stormwater Samples for Measurement of Dissolved Metals

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Suggested Citation:"Appendix B - Detailed Cleaning Protocol for Equipment to be Used for Collection of Stormwater Samples for Measurement of Dissolved Metals." National Academies of Sciences, Engineering, and Medicine. 2014. Measuring and Removing Dissolved Metals from Stormwater in Highly Urbanized Areas. Washington, DC: The National Academies Press. doi: 10.17226/22389.
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Suggested Citation:"Appendix B - Detailed Cleaning Protocol for Equipment to be Used for Collection of Stormwater Samples for Measurement of Dissolved Metals." National Academies of Sciences, Engineering, and Medicine. 2014. Measuring and Removing Dissolved Metals from Stormwater in Highly Urbanized Areas. Washington, DC: The National Academies Press. doi: 10.17226/22389.
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Suggested Citation:"Appendix B - Detailed Cleaning Protocol for Equipment to be Used for Collection of Stormwater Samples for Measurement of Dissolved Metals." National Academies of Sciences, Engineering, and Medicine. 2014. Measuring and Removing Dissolved Metals from Stormwater in Highly Urbanized Areas. Washington, DC: The National Academies Press. doi: 10.17226/22389.
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Suggested Citation:"Appendix B - Detailed Cleaning Protocol for Equipment to be Used for Collection of Stormwater Samples for Measurement of Dissolved Metals." National Academies of Sciences, Engineering, and Medicine. 2014. Measuring and Removing Dissolved Metals from Stormwater in Highly Urbanized Areas. Washington, DC: The National Academies Press. doi: 10.17226/22389.
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Suggested Citation:"Appendix B - Detailed Cleaning Protocol for Equipment to be Used for Collection of Stormwater Samples for Measurement of Dissolved Metals." National Academies of Sciences, Engineering, and Medicine. 2014. Measuring and Removing Dissolved Metals from Stormwater in Highly Urbanized Areas. Washington, DC: The National Academies Press. doi: 10.17226/22389.
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Suggested Citation:"Appendix B - Detailed Cleaning Protocol for Equipment to be Used for Collection of Stormwater Samples for Measurement of Dissolved Metals." National Academies of Sciences, Engineering, and Medicine. 2014. Measuring and Removing Dissolved Metals from Stormwater in Highly Urbanized Areas. Washington, DC: The National Academies Press. doi: 10.17226/22389.
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Suggested Citation:"Appendix B - Detailed Cleaning Protocol for Equipment to be Used for Collection of Stormwater Samples for Measurement of Dissolved Metals." National Academies of Sciences, Engineering, and Medicine. 2014. Measuring and Removing Dissolved Metals from Stormwater in Highly Urbanized Areas. Washington, DC: The National Academies Press. doi: 10.17226/22389.
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Suggested Citation:"Appendix B - Detailed Cleaning Protocol for Equipment to be Used for Collection of Stormwater Samples for Measurement of Dissolved Metals." National Academies of Sciences, Engineering, and Medicine. 2014. Measuring and Removing Dissolved Metals from Stormwater in Highly Urbanized Areas. Washington, DC: The National Academies Press. doi: 10.17226/22389.
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Suggested Citation:"Appendix B - Detailed Cleaning Protocol for Equipment to be Used for Collection of Stormwater Samples for Measurement of Dissolved Metals." National Academies of Sciences, Engineering, and Medicine. 2014. Measuring and Removing Dissolved Metals from Stormwater in Highly Urbanized Areas. Washington, DC: The National Academies Press. doi: 10.17226/22389.
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Suggested Citation:"Appendix B - Detailed Cleaning Protocol for Equipment to be Used for Collection of Stormwater Samples for Measurement of Dissolved Metals." National Academies of Sciences, Engineering, and Medicine. 2014. Measuring and Removing Dissolved Metals from Stormwater in Highly Urbanized Areas. Washington, DC: The National Academies Press. doi: 10.17226/22389.
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Suggested Citation:"Appendix B - Detailed Cleaning Protocol for Equipment to be Used for Collection of Stormwater Samples for Measurement of Dissolved Metals." National Academies of Sciences, Engineering, and Medicine. 2014. Measuring and Removing Dissolved Metals from Stormwater in Highly Urbanized Areas. Washington, DC: The National Academies Press. doi: 10.17226/22389.
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Suggested Citation:"Appendix B - Detailed Cleaning Protocol for Equipment to be Used for Collection of Stormwater Samples for Measurement of Dissolved Metals." National Academies of Sciences, Engineering, and Medicine. 2014. Measuring and Removing Dissolved Metals from Stormwater in Highly Urbanized Areas. Washington, DC: The National Academies Press. doi: 10.17226/22389.
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Suggested Citation:"Appendix B - Detailed Cleaning Protocol for Equipment to be Used for Collection of Stormwater Samples for Measurement of Dissolved Metals." National Academies of Sciences, Engineering, and Medicine. 2014. Measuring and Removing Dissolved Metals from Stormwater in Highly Urbanized Areas. Washington, DC: The National Academies Press. doi: 10.17226/22389.
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Suggested Citation:"Appendix B - Detailed Cleaning Protocol for Equipment to be Used for Collection of Stormwater Samples for Measurement of Dissolved Metals." National Academies of Sciences, Engineering, and Medicine. 2014. Measuring and Removing Dissolved Metals from Stormwater in Highly Urbanized Areas. Washington, DC: The National Academies Press. doi: 10.17226/22389.
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Suggested Citation:"Appendix B - Detailed Cleaning Protocol for Equipment to be Used for Collection of Stormwater Samples for Measurement of Dissolved Metals." National Academies of Sciences, Engineering, and Medicine. 2014. Measuring and Removing Dissolved Metals from Stormwater in Highly Urbanized Areas. Washington, DC: The National Academies Press. doi: 10.17226/22389.
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Below is the uncorrected machine-read text of this chapter, intended to provide our own search engines and external engines with highly rich, chapter-representative searchable text of each book. Because it is UNCORRECTED material, please consider the following text as a useful but insufficient proxy for the authoritative book pages.

B-1 A P P E N D I X B Detailed Cleaning Protocol for Equipment to be Used for Collection of Stormwater Samples for Measurement of Dissolved Metals

B-2 CLEANING PROTOCOL FOR: FEP intake sampling hoses, silicon peristaltic pump tubing, and sub-sampling hose setups. 1.0 SCOPE This Standard Operating Procedure (SOP) describes the procedures required to properly clean hoses and tubing involved in non-point source (NPS) sampling. These include: The purpose of these procedures is to ensure contaminant-free sampling hoses and to ensure the safety of the personnel performing these procedures. 2.0 APPLICATION This SOP applies to all activities pertaining to the cleaning of NPS sampling hoses. 3.0 HEALTH AND SAFETY CONSIDERATIONS The cleaning of sampling hoses may subject personnel performing this task to contact with hazardous materials. Skin contact with all materials and solutions should be minimized by wearing appropriate personal protective equipment (PPE) including: chemically-resistant protective gloves, laboratory coats, chemically-resistant aprons and goggles. In addition, the material safety data sheets (MSDSs) for nitric acid and laboratory detergents should be reviewed prior to beginning this task to ensure that you are aware of the hazards involved with handling the respective chemicals as well as being informed of any revisions to the data sheets. When introducing soap or acid through a series of hose with a peristaltic pump, it is safest to “Pull” the fluids through vs. “Push”. Pushing the fluids through may over- pressurize the connections and blow out (particularly if there is an obstruction, e.g., twisted hose, kink, etc.). Pulling the fluids through the series creates a negative pressure inside the tubing and reduces the potential for accidents. 4.0 DEFINITIONS 4.1 Tubing - either sample intake hose, sub-sample hose, or peristaltic pump tubing. 4.2 Intake sampling hose - 3/8" I.D. x 1/2" O.D. FEP tubing. 4.3 Sub-sampling hose setup - two 3-4 foot sections of 3/8-inch I.D. x 1/2-inch O.D. FEP hose connected with a section of silicon peristaltic pump tubing. 4.4 Peristaltic pump tubing - 3/8" I.D. x 5/8" O.D. silicon tubing. 4.5 DI water - commercial de-ionized water. 4.6 Laboratory Detergent - 2% solution of Contrad 70® or Micro-90® detergent.

B-3 5.0 EQUIPMENT 5.1 Instrumentation: 1) Peristaltic pump 5.2 Reagents: 1) ACS Reagent Grade nitric acid in a 2 Normal solution (2N HNO3) 2) Contrad 70® non-phosphate laboratory detergent 3) Micro-90® non-phosphate laboratory detergent 4) Baking soda or equivalent to neutralize acid 5) pH paper 5.3 Apparatus: 1) Numerous 4-inch sections of protocol-cleaned silicon tubing. 2) Numerous 4-inch sections of protocol-cleaned Teflon® tubing. 3) Protocol-cleaned polyethylene bucket with lid (with hole in top). 4) Neutralization tank. 5.4 Documentation: Label each hose as to the date each was cleaned and the initials of the cleaning technician. 6.0 CLEANING PROCEDURES. Care must be taken to ensure that no contaminants are introduced at any point during these procedures. If the wash is not performed with this in mind, the possibility for the introduction of contaminants (i.e., from dirty floors, dirty counter tops, dirty fingers/gloves, dirty hose ends, etc.) is increased significantly. 6.1 Sub-sampling Hose Setup: 6.1.0 This is used with a peristaltic pump to sub-sample from a 20 liter composite sample bottle and to facilitate pumping and/or circulation of laboratory detergent and nitric acid. A sub-sampling hose setup consists of two lengths of FEP hose (one approximately 3 feet and the other 4 feet) connected by a 24-inch section of silicon tubing. Numerous sub-sampling hose setups should be cleaned simultaneously by connecting them by 4-inch

B-4 sections of silicon peristaltic tubing. Important: Check for kinks or twists along the series that would inhibit the flow in and out. 6.1.1 48 Hour Soak: Place the series of hoses to be cleaned into a secondary container until the entire washing process is completed. Prepare a 2% solution of laboratory detergent in a protocol-cleaned bucket. Install one sub-sampling hose setup into a peristaltic pump. Connect this with the series of sub-sampling hose setups using a 4-inch section of silicon peristaltic tubing. Pump the detergent solution into the series of sub- sampling hose setups. It is recommended that the fluids be “pulled” through vs. “pushed”. Circulate the solution through the hoses and bucket until there are no air bubbles left in the hoses. Separate both ends of the hose series from the pump setup and cap them with protocol-cleaned orange caps OR connect both ends using a protocol-cleaned 4-inch section of silicon. Let the hose soak for 48 hours. Pump out detergent solution and dispose of used solution down a sanitary drain. 6.1.2 Tap Water Rinse: Rinse by pumping tap water for 5 minutes from a protocol-cleaned HDPE bucket through the hose/hoses and into a neutralization tank and dispose of the rinsate in a sanitary drain. Important: In order to avoid contaminating the rinse water always be sure to clean the outside of the hose end that will be immersed in the rinse water: wash with laboratory detergent and a plastic brush, rinse with tap water and rinse three times with DI water. 6.1.3 DI Water Rinse: Rinse by pumping DI water for 5 minutes from a protocol-cleaned HDPE bucket through the hose/hoses and into a neutralization tank and dispose of the rinsate in a sanitary drain. 6.1.4 2N (10%) Nitric Acid (2N HNO3) Wash: Wash with 2N (10%) nitric acid solution by pumping in a circular cycle for 10 minutes from the 2N (10%) nitric acid carboy. Do not exceed 10 minutes. Pump all the acid back into the acid carboy. 6.1.5 DI Water Rinse: Rinse by pumping DI water through the hose into the neutralization tank for 7 minutes. Neutralize and dispose of rinsate in accordance with all federal, state, and local regulations 6.1.6 FEP Hose and Peristaltic Tubing Storage: To store FEP hose put protocol-cleaned orange polypropylene caps on each end. To secure the silicon peristaltic tubing, attach both ends with a small protocol cleaned piece of FEP hose. Store the hose or tubing in a new garbage bag to

B-5 prevent contamination before use. Label as clean, the date cleaned, and your initials. 6.1.7 Sub-Sampling Hose Exterior Cleaning and Storage: NPS sub-sampling hoses require an additional cleaning procedure for the exterior portions of the hose (approximately 2 feet on one end) using protocol-cleaned squirt bottles as follows: 1) Place a protocol-cleaned orange cap on one end of the sub- sampling hose and wash the remaining end with a 2% solution of laboratory detergent using a plastic brush. Hold the hose in a way that prevents interior contamination from the exterior cleaning procedure. 2) Rinse end three times with tap water. 3) Rinse end three times with DI water. 4) Wash end three times with 2N nitric acid squirt bottle. 5) Rinse end three times again with DI water. Dispose of rinsate in accordance with all federal, state, and local regulations. 6) Place a protocol-cleaned orange cap on the end and cover with a long plastic bag. Secure bag with a rubber band. Store the tubing in a new large plastic bag to prevent contamination before use. Label as clean, the date cleaned, and your initials.

B-6 CLEANING PROTOCOL FOR: Miscellaneous Laboratory Equipment used for Cleaning and Blanking 1.0 SCOPE This Standard Operating Procedure describes the procedures for cleaning the miscellaneous items necessary to complete the tasks of cleaning 20-liter composite sample bottles and hoses. The purpose of these procedures is to ensure that the items are contaminant free and to ensure the safety of the personnel performing this procedure. 2.0 APPLICATION This SOP applies to all laboratory activities that comprise the cleaning of ancillary items necessary to complete the tasks of cleaning 20 liter composite sample bottles and NPS hoses. 3.0 HEALTH AND SAFETY CONSIDERATIONS The cleaning of the following items may involve contact with hazardous materials. Skin contact with all materials and solutions should be minimized by wearing appropriate personal protective equipment (PPE) including: chemically-resistant protective gloves, laboratory coats, chemically-resistant aprons, and goggles. In addition, to ensure that you are aware of the hazards involved and of any new revisions to the procedure, the material safety data sheets (MSDSs) for nitric acid and the laboratory detergent should be reviewed before beginning any of these procedures. 4.0 DEFINITIONS 4.1 Polyethylene Squirt Bottles - ½ and 1 liter squirt bottles for washing and/or rinsing with DI water or nitric acid. 4.2 Polycarbonate and Polyethylene De-ionized Water Jugs - For holding DI water. 4.3 Polyethylene Bucket - For holding tap water, DI water or detergent solutions during hose washing procedures. 4.4 Four-inch Teflon® Connector - For connecting two lengths of silicon peristaltic tubing together. 4.5 Four-inch Silicon Connector - For connecting two lengths of Teflon® hose together. 4.6 Orange Polypropylene Hose Caps - For placing over the ends of clean Teflon® hose to prevent contamination.

B-7 4.7 De-ionized (DI) water - Commercial de-ionized water. 4.8 Laboratory Detergent - 2% solution of Contrad 70® or Micro-90® detergent. 5.0 EQUIPMENT 5.1 Instrumentation: Not applicable. 5.2 Reagents: 1) ACS Reagent Grade nitric acid as a 2 Normal solution (2N HNO3). 2) Micro-90® non-phosphate laboratory detergent. 3) Contrad 70® non-phosphate laboratory detergent. 4) Contrad 70® anti-foaming agent. 5) pH paper or pH meter. 6) Baking soda (NaHCO3), marble chips or equivalent to neutralize acid 5.3 Apparatus: 1) Clean polyethylene squirt bottles. 2) Clean polyethylene trays or 2000 ml glass beakers. 3) Neutralization Tank. 5.4 Documentation: Label each squirt bottle, DI jug, storage container holding clean items, etc., as to the date each was cleaned and the initials of the cleaning technician. 6.0 CLEANING PROCEDURES Care must be taken to ensure that no contaminants are introduced at any point during these procedures. If the wash is not performed with this in mind, the possibility for the introduction of contaminants (i.e., from dirty sinks, dirty counter tops, dirty fingers/gloves, dirty hose ends, etc.) is increased significantly. Rinsing properly is essential to ensure proper cleaning. This is done by squirting the liquid over the item to be cleaned in a top-down fashion, letting the water flow off completely before applying the next rinse. Rinse the item in this fashion a minimum of three times. Numerous rinses of relatively small volumes are much better than one or two rinses of higher volume. Be aware of handling: use clean gloves (it is best if they have gone through the same prior wash as the item to be rinsed) and rinse off the fingers prior to grasping the item to be cleaned. Try to

B-8 grasp the item in a slightly different place between rinses so one’s fingers do not cover a portion of the item throughout the rinses. 6.1 Polyethylene squirt bottles: 1) Soak in a 2% solution of laboratory detergent in a protocol-cleaned bucket for 48 hours. 2) Rinse thoroughly (minimum of three times) with tap water. 3) Rinse thoroughly (minimum of three times) with DI water. 4) Wash three times with 2N (10%) nitric acid. 5) Rinse thoroughly (minimum of three times) with DI water. Neutralize and dispose of rinsate in accordance with all federal, state, and local regulations. 6.2 Polycarbonate and Polyethylene DI Water Jugs: 1) Fill to the rim with a 2% solution of laboratory detergent, cap the jug, and let soak for 48 hours. Wash cap with an all-plastic scrub brush after soak. 2) Rinse thoroughly (minimum of three times) with tap water. 3) Rinse thoroughly (minimum of three times) with DI water. 4) Wash three times with 2N (10%) nitric acid. 5) Rinse thoroughly (minimum of three times) with DI water. Neutralize and dispose of rinsate in accordance with all federal, state, and local regulations. 6.3 Polyethylene Bucket: 1) Fill to the rim with a 2% solution of laboratory detergent and let soak for 48 hours. 2) Rinse thoroughly (minimum of three times) with tap water. 3) Rinse thoroughly (minimum of three times) with DI water. 4) Wash three times with 2N (10%) nitric acid squirt bottle. 5) Rinse thoroughly (minimum of three times) with DI water. Neutralize and dispose of rinsate in accordance with all federal, state, and local regulations. Label as to the date cleaned and initial.

B-9 6.4 Four-inch Teflon® and Silicon Hose Connectors and Orange Polypropylene Hose Caps. The purpose of the four-inch sections of Teflon® and silicon hose is to connect longer lengths of each type of hose together during the hose cleaning procedures. The orange polypropylene hose caps are for the ends of cleaned FEP hoses to prevent contamination prior to use in the field or laboratory. 1) Using a 2% solution of laboratory detergent, soak the four-inch sections of FEP hose, silicon tubing, and orange caps for 48 hours. 2) Rinse thoroughly with tap water (minimum of three rinses). 3) Rinse thoroughly with DI water (minimum of three rinses). 4) Using a squirt bottle filled with 2N (10%) HNO3, thoroughly rinse the interior and exterior of the connectors and caps thoroughly OR, roll/agitate them in a shallow layer of 2N (10%) HNO3 in a laboratory detergent cleaned glass beaker or other appropriate, clean container for a more thorough washing. 5) Thoroughly rinse connectors and caps with DI water (minimum of three rinses). Neutralize and dispose of rinsate in accordance with all federal, state, and local regulations. Keep clean connectors and caps in a similarly cleaned (or certified clean) widemouth glass jar or detergent-cleaned resealable bag and label as clean, date cleaned, and initial.

B-10 CLEANING PROTOCOL FOR: 20-L Borosilicate Glass Composite Bottles (Media Bottles) and Closures 1.0 SCOPE This Standard Operating Procedure (SOP) describes the procedures for the cleaning of 20-liter composite sample bottles and the related equipment necessary to complete the task. The purpose of these procedures is to ensure that the sample bottles are contaminant-free and to ensure the safety of the personnel performing this procedure. 2.0 APPLICATION This SOP applies to all laboratory activities that comprise the cleaning of 20-liter composite sample bottles and stoppers. 3.0 HEALTH AND SAFETY CONSIDERATIONS The cleaning of 20-liter composite-sample bottles and associated equipment involves hazardous materials. Skin contact with all materials and solutions should be minimized by wearing appropriate personal protective equipment (PPE) including: chemical- resistant gloves, laboratory coats, chemical-resistant aprons, and goggles. To ensure that you are aware of the hazards involved, the material safety data sheets (MSDSs) for nitric acid and laboratory detergents should be reviewed before beginning any of these procedures. Note: Preparations should be made to contain and neutralize any spillage of acid. Be aware of the location of absorbent, neutralizing, and containment materials in the bottle cleaning area. 4.0 DEFINITIONS 4.1 Composite sample bottle - 20 liter borosilicate glass bottle that is used with autosamplers to collect a stormwater composite sample. 4.2 Stopper - a Teflon® cap used to seal the composite sample bottle (either solid or drilled with holes for the silicon inlet tubing). 4.3 O-Ring - Viton O-ring 23/8"- I.D. x 23/4"- O.D. that is located around the base of stopper. 4.4 Clamp - Polypropylene clamp, 2 bolts, and wing nuts specifically designed to fasten the stopper and the O-ring to the rim of the composite sample bottle. 4.5 De-ionized (DI) water - commercial de-ionized water (12-13 Megohm/cm).

B-11 4.6 Laboratory Detergent - 2% solution of Contrad 70® or Micro-90® detergent. 5.0 EQUIPMENT 5.1 Instrumentation: 1) Peristaltic pump with a protocol-cleaned sub-sampling hose setup. 5.2 Reagents: 1) ACS Reagent Grade nitric acid in a 2 Normal solution (2N HNO3) 2) Contrad 70® non-phosphate laboratory detergent 3) Contrad 70® anti-foaming agent 4) Micro-90® non-phosphate laboratory detergent 5) Baking soda or equivalent to neutralize acid 6) pH paper 5.3 Apparatus: 1) Bottle Rolling Rack 2) DI Rinse Rack 3) Yellow Neutralization Drip Bucket 4) Neutralization Tank 5.4 Documentation: The status of each composite sample bottle must be tracked. Bottles should be washed in batches of 10, 20, or 30 and the status of each batch must be made apparent to all personnel by posting a large status label (including the start date) with each batch. This will ensure that all required soak times have been attained and that each bottle was subjected to the proper cleaning procedures. Information on each batch of bottles cleaned (including bottle number, QA batch, date cleaning started, date finished, date blanked, and cleaning technicians) should be entered in the Bottle Cleaning Log Sheet. 6.0 CLEANING PROCEDURES Care must be taken to ensure that no contaminants are introduced at any point during this procedure. If the wash is not performed with this in mind, the possibility for the

B-12 introduction of contaminants (i.e., from dust, dirty sub-sampling tubing tips, dirty fingers/gloves, automobile emissions, etc.) is increased significantly. 6.1 Teflon® Bottle Stoppers with/without Holes and Field Extras: To be performed whenever required for field use. 1) Wash with laboratory detergent using a clean all-plastic brush. 2) Rinse thoroughly (minimum of three times) with tap water. 3) Rinse thoroughly (minimum of three times) with DI water. 4) Wash three times with 2N nitric acid squirt bottle. 5) Rinse thoroughly (minimum of three times) with DI water. 6) Allow to dry in a dust-free environment. 7) Store in two sealed clean Ziploc® bags. 6.2 NPS 20-Liter Composite Sample Bottle Cleaning: 6.2.1 Preliminary Bottle Cleaning: Bottles should undergo a preliminary rinse with tap water as soon as possible after they are available. This includes dumping any remaining stormwater into a sanitary drain and rinsing the bottles and stoppers. This prevents material from adhering to the interior surface of the bottle. 6.2.2 48 Hour Soak: Place the bottle to be cleaned into a secondary containment bucket. Prepare a 2% solution of laboratory detergent with tap water directly in the bottle. Note: Since laboratory detergent is a foaming solution, add 3/4 of the tap water first, add the detergent, then add the rest of the water. Should excessive foam be generated, a few drops of Contrad 70® anti-foaming agent may be added. Make sure that the bottle is filled to the rim and scrub the rim with an all-plastic scrub brush. Scrub a Teflon® stopper with 2% solution of laboratory detergent and place stopper over the full bottle so overflowing happens. This will allow both the stopper and the bottle to soak for 48 hours. After the 48 hour soak, this solution may be may be retained for reuse (i.e., siphoned into other dirty bottles) or it can be poured off into a sanitary drain. 6.2.3 Tap-Water Rinse: Tap water rinses detergent better than DI water. Flush upside down bottle with tap water for 20 sec. Rinse each bottle 3 times with tap water being careful not to contaminate the clean surfaces.

B-13 6.2.4 DI Rinse: Rinse the top and neck of the bottles with DI water using a squirt bottle and then rinse upside down for three minutes on the DI rinse rack for bottles. Make sure to tip bottles from side to side for a more thorough rinsing. Allow 1-2 minutes for the bottles to drain as much as possible. Rinse each stopper with DI water squirt bottle 3 times (being careful not to touch the clean surfaces). 6.2.5 Acid Wash: Note that it is important to wash the bottle with 2N nitric acid according to the following procedure: 1) Place the empty bottle near the 2N nitric acid carboy and peristaltic pump. The location should be able to safely contain a spill if the 20-liter bottle breaks. 2) Pump acid into the bottle using the peristaltic pump fitted with a protocol- cleaned sub-sampling hose setup. 3) Fill the bottle slightly more than half full. 4) Place a protocol-cleaned solid Teflon® stopper (with a properly seated O- ring) (refer to Section 6.2.3 above) on the bottle and clamp it securely. 5) Carefully lift and place the bottle on the roller rack and check for leakage from the stopper. Neutralize any spillage. Often small leaks can be corrected by a slight tightening of the clamp. Roll the bottles for twenty minutes. 6) Pump the acid into another bottle for rolling or back into the 2N nitric acid carboy. 6.2.6 DI Rinse for Bottles: Allow the bottles to drain into a yellow neutralization bucket for at least 1 minute. Place four bottles at a time on the DI rinse rack and rinse for 5 minutes. Move bottles around to ensure complete and thorough rinsing. Rinse the outside of the bottle with tap water. Allow bottles to drain for 2 minutes. 6.3 Storage: Clamp a stopper (one that went through the entire cleaning procedure) on the bottle. Properly label the bottle as to the date cleaned and by whom and place on the bottle storage rack or in a secondary containment bucket in a safe area. Also, fill out the Bottle Cleaning Log Sheet. 7.0 QUALITY ASSURANCE REQUIREMENTS 7.1 The 20-liter composite sample bottles must be evaluated (“blanked”) for contaminants after they have completed the decontamination procedure. The analytical laboratory performing the evaluation should supply Milli-Q® water that is used as a blanking rinsate, and sample bottles for the appropriate constituents of

B-14 concern. This evaluation will be accomplished by randomly blanking 10% of the washed bottles, or 1 bottle per batch (whichever is greater) and having the blanking rinsate analyzed by the laboratory for the appropriate constituents. 7.2 If any of the bottles fail the analyses (concentration of any analytes are at or above the limit of detection), all of the bottles from that batch must be decontaminated. Again, 10% of these bottles must be subjected to the blanking process as described above. 7.3 If results of the evaluation process show that the bottles are not contaminant-free, the cleaning procedure must be re-evaluated. Consult with the Quality Assurance/Quality Control Officer to determine the source of contamination.

Abbreviations and acronyms used without definitions in TRB publications: A4A Airlines for America AAAE American Association of Airport Executives AASHO American Association of State Highway Officials AASHTO American Association of State Highway and Transportation Officials ACI–NA Airports Council International–North America ACRP Airport Cooperative Research Program ADA Americans with Disabilities Act APTA American Public Transportation Association ASCE American Society of Civil Engineers ASME American Society of Mechanical Engineers ASTM American Society for Testing and Materials ATA American Trucking Associations CTAA Community Transportation Association of America CTBSSP Commercial Truck and Bus Safety Synthesis Program DHS Department of Homeland Security DOE Department of Energy EPA Environmental Protection Agency FAA Federal Aviation Administration FHWA Federal Highway Administration FMCSA Federal Motor Carrier Safety Administration FRA Federal Railroad Administration FTA Federal Transit Administration HMCRP Hazardous Materials Cooperative Research Program IEEE Institute of Electrical and Electronics Engineers ISTEA Intermodal Surface Transportation Efficiency Act of 1991 ITE Institute of Transportation Engineers MAP-21 Moving Ahead for Progress in the 21st Century Act (2012) NASA National Aeronautics and Space Administration NASAO National Association of State Aviation Officials NCFRP National Cooperative Freight Research Program NCHRP National Cooperative Highway Research Program NHTSA National Highway Traffic Safety Administration NTSB National Transportation Safety Board PHMSA Pipeline and Hazardous Materials Safety Administration RITA Research and Innovative Technology Administration SAE Society of Automotive Engineers SAFETEA-LU Safe, Accountable, Flexible, Efficient Transportation Equity Act: A Legacy for Users (2005) TCRP Transit Cooperative Research Program TEA-21 Transportation Equity Act for the 21st Century (1998) TRB Transportation Research Board TSA Transportation Security Administration U.S.DOT United States Department of Transportation

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TRB’s National Cooperative Highway Research Program (NCHRP) Report 767: Measuring and Removing Dissolved Metals from Stormwater in Highly Urbanized Areas presents prototype best management practices (BMPs) for the removal of dissolved metals in stormwater runoff.

The report presents three conceptual configurations in detail: two vault system configurations for urban and rural settings, and an inlet scupper with media for bridge deck drainage systems.

The report also includes standard protocols to accurately measure the levels of dissolved metals in stormwater. Practical guidance on the use of these protocols is provided in an appendix to the final report. The report is accompanied by an Excel spreadsheet on CD designed to assist in sizing the filter bed in the vaults and the bridge deck inlet scupper.

The CD is also available for download from TRB’s website as an ISO image. Links to the ISO image and instructions for burning a CD from an ISO image are provided below.

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CD Disclaimer - This software is offered as is, without warranty or promise of support of any kind either expressed or implied. Under no circumstance will the National Academy of Sciences or the Transportation Research Board (collectively "TRB") be liable for any loss or damage caused by the installation or operation of this product. TRB makes no representation or warranty of any kind, expressed or implied, in fact or in law, including without limitation, the warranty of merchantability or the warranty of fitness for a particular purpose, and shall not in any case be liable for any consequential or special damages.

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