Attachment 01 - NIH Metals.1714658452634.docx

Attachment 01 – NIH Metals (Cations-Ion Chromotography) Summary The analysis described in this method involves multi-elemental determinations by ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectroscopy) or ICP-MS (Inductively Coupled Plasma-Mass Spectroscopy) using sequential or simultaneous instruments. The instruments measure characteristic atomic-line emission spectra by optical spectrometry. Samples are nebulized and the resulting aerosol is transported to the plasma torch. Element specific emission spectra are produced by a radiofrequency inductively coupled plasma. The spectra are dispersed by a grating spectrometer, and the intensities of the line spectra are monitored at specific wavelengths by a photosensitive device.

Sample Collection NIH shall collect samples, and the Contractor shall pick up the samples from NIH Bethesda, Building 11. The Contractor shall provide NIH with sampling kits for collecting each sample. Please note that special sample collection procedures may apply for copper (NPDES). Comment by Hughes, Casey (NIH/OD/ORF) [E]: Do labs use sampling kits or use their own materials? Comment by Adjei, George (NIH/OD/ORF) [E]: Lab use sampling kits The Contractor’s personnel assigned to pick up the samples shall be trained in sampling procedures and they shall adhere to the correct procedures for sample collection, sample preservation, sample handling, sample identification, and prompt transfer of the sample to the laboratory. The laboratory shall inspect samples and accompanied paperwork (e.g. chain of custody documents) and reject samples that are not collected in accordance with applicable procedures.

In the event that the Contractor also collects the sample, they shall follow the following procedure:

When total and dissolved metals analysis is required, collect sample in two 250-mL containers or one 500-mL container. Fill a prepared 250 mL, 500 mL, 1000 mL, or 2000 ML bottle as applicable from a free-flowing sample tap or other sources as applicable. Minimize air bubbles and fill the bottle almost but not completely to allow room for nitric acid preservative addition at the lab. The volume of sample collected shall be sufficient to ensure a representative sample, allow for replicate analysis and laboratory fortified matrix analysis, if required, and minimize waste disposal

Sample Preservation and Storage Preservation with nitric acid is required for elemental analysis by ICP-MS and ICP-AES. If the sample is not field-preserved, it shall be preserved upon receipt at the laboratory with concentrated nitric acid (optima grade) so that the sample has a 1% nitric acid matrix (2.5 mL nitric acid is added to 250 mL of sample). Samples shall be returned to the laboratory within two weeks of collection. Comment by Hughes, Casey (NIH/OD/ORF) [E]: Suggest we decide if field-preserved or lab preserved rather than provide option Comment by Adjei, George (NIH/OD/ORF) [E]: It depends, some sample bottles come with preservation in it.

Once a sample is preserved with nitric acid, samples shall be stored at room temperature with every effort taken to keep the sample from temperature extremes. If elemental analysis samples are shipped, they do not need to be iced again, but they shall be kept from temperature extremes. A thermally insulated sampling kit, designed to fit sampling bottles securely during shipment, shall be used to protect the samples from these temperature extremes.

Samples shall be well mixed with the acid preservative, and they shall be stored for 16 hours at room temperature prior to checking them for pH and turbidity. If the check reveals pH to be greater than 2, additional acid must be added to lower the pH to <2 and held for additional 16 hours until verified to be pH <2. If the turbidity is >1 NTU, schedule the sample for analysis after acid digestion.

For the determination of dissolved elements, the sample must be filtered through a 0.45 μm pore diameter membrane filter at the time of collection or as soon thereafter as practically possible.

Method of Shipping and Duration The Contractor shall chill the sample to 4° C prior to shipping and ensure that sample temperature is maintained at 4° C until nitric acid preservation in the lab prior to analysis. Filtration and preservation may be done in the field at the time of collection. However, to avoid the hazards of strong acids in the field, transport restrictions, and possible contamination, it is recommended that the samples be returned to the laboratory within two weeks of collection, filtered if not filtered in the field and acid preserved upon receipt in the laboratory.

Procedure of their receipt and storage If properly acid preserved, the sample can be held up to 6 months before analysis. The sample shall be received with a chain of custody (COC), The COC shall have the name of the sample collector, date and time of sample collection, signature or initial of the sample collector, location of the sample and type of sample to be analyzed.

Lab Procedure for Analysis Metals determination shall be performed using ICP-MS or ICP-AES. All samples, blanks, spikes, and standards must be analyzed using the same procedure under identical conditions. Instrument shall be tuned and calibrated daily, and the samples shall be characterized, and digested, if necessary, prior to instrumental analysis. Comment by Hughes, Casey (NIH/OD/ORF) [E]: What is our requirement as far as method? Comment by Adjei, George (NIH/OD/ORF) [E]: Any of the 3 instruments will be fine

Maintenance plan for the instrument The Contractor shall perform maintenance on their equipment as outlined per the manufacturer’s instructions.

The maintenance protocol shall be available and be delivered to NIH upon request.

Calibration Procedure The daily instrument setup, pre-calibration routine, initial calibration, and continuing calibration verification, etc. shall be performed each day samples are analyzed. The analyst shall follow the recommended operating conditions provided by the manufacturer. It is the responsibility of the analyst to verify that the instrument configuration and operating conditions satisfy the analytical requirements and to maintain quality control data verifying instrument performance and analytical results Comment by Hughes, Casey (NIH/OD/ORF) [E]: Suggest to include in Quality Control Section of SOW rather than each appendix Comment by Adjei, George (NIH/OD/ORF) [E]: It depends on the methods each appendix uses

Analysis Method and Protocol The analysis method shall be based on EPA method 200.7 and 200.8

References EPA Method 200.7, Determination of Trace Elements in Water and Wastes by Inductively Coupled Plasma Atomic Emission Spectrometry, Revision 4.4,1994.

EPA Method 200.8, Determination of Trace Elements in Water and Wastes by Inductively Coupled Plasma Mass Spectrometry, Revision 5.4, 1994.

USEPA Manual for the Certification of Laboratories Analyzing Drinking Water (CLDW), Fifth Edition, EPA 815-R-05-004, January 2005.

Supplement 1 to the Fifth Edition of the Manual for the Certification of Laboratories Analyzing Drinking Water, EPA 815-F-08-006, June 2008