Attachment_2_-_Quality_Assurance_Surveillance_Plan_for_Testing.pdf

Attachment 2 - Quality Assurance Surveillance Plan (QASP) for Testing

1. Acid, vial (PP), HNO3, 7.5N, 2 mL Ultrex

Quality Assurance (QA) procedure, performed by QAS (Quality Assurance Section) personnel:

• There are two components to these vials – the acid and the container. If a new lot of vials are to be tested and the acid is of a previously approved acid lot, only 1 new vial is tested with another vial from an approved lot. If either the acid or container is of an untested lot, the QA study will typically consist of 8 vials from the new lot and 1 vial from an approved lot.

• Obtain 3 randomly selected boxes of (24 vials/box) from Support Services (SS). Also, select 1 vial of acid from a currently approved lot (usually in stock in the QAS laboratory) to be the control sample. Make sure the control lot is not expired. Contact

SHE (Safety, Health and Environmental section) for disposal of expired acids.

• Rinse previously approved FA bottles and caps 3 times with Nanopure water. Fill each bottle to about the shoulder with Nanopure water and cap the bottle.

• Place bottles in fume hood and to each of the bottles designated for the new acid lot, add

1 vial of 7.5N-7.7N 2mL HNO3 from the new lot. From an approved acid lot, add 1 vial to the designated control sample. Note the acid lots in the NFSS QA logbook. Recap the bottles and set them aside. Dispose of the acid vials and caps in the solid trace acid waste container.

• Label bottles with the following information: Station ID, date, time, and bottle type.

(Label templates may be found at Archie > qas > NFSS(all files) > NFSS ASRs &

Labels.) Samples are logged in for analysis by LS2048 (Metals by ICP and ICP-MS).

• Place a round “RUSH” label on the cap of each bottle. (Login will provide the labels as needed.)

Lot acceptance criteria:

• If all data are reported below the reporting limits for all the constituents in all the samples, the QAS analyst emails SS with approval for sale (see the QASP for email convention details).

• If the data indicate possible contamination with values at or above the reporting limits, a request for verification of rerun information for that data will be made by QAS to the appropriate group. If the data verify below the reporting limits, the QAS analyst emails SS with approval for sale.

• If the data verify at or above the reporting limits, repeat the QA procedure for that (those) constituents.

• If the data indicate sporadic problems for an analyte in the material, then a note will be included on the certificate of analysis that indicates the extent of the problem.

• If the material is determined to be unacceptable, the QAS NFSS (Quality Assurance

Section National Field Supply Service) staff will meet with SS personnel to determine the next course of action. This may include returning the material to the vendor.

2. Acid, Vial (PP), H2SO4, 4.5N (1:7), 1 mL, WCA, Nutrient/carbon

QA procedure, performed by QAS personnel:

• Determine the number of samples to be included in the quality assurance study. There are two components to these vials – the acid and the container. If a new lot of vials are to be tested and the acid is of a previously approved acid lot, only one new vial is tested with another vial from an approved lot. If either the acid or container is of an untested lot, the QA study will typically consist of 9 vials from the new lot and 2 vials from an approved lot.

Note: Two bottle types are required for QA testing this acid ‒ FCA (Filtered

Chilled Acidified) and DOC (Dissolved Organic Carbon). A study will consist of one of the following QA sets depending on whether the acid lot has been previously approved:

1 FCA + 1 DOC + 1 FCA control + 1 DOC control Previously approved acid lot or 9 FCA + 9 DOC + 1 FCA control + 1 DOC control New acid lot

• Obtain 3 randomly selected boxes of (24 vials/box) from Support Services (SS), one from each shipping box. Also, select 2 vials of acid (one for each bottle type) from a currently approved lot (usually in stock in the QAS laboratory) to be the control sample. Make sure the control lot is not expired. Contact SHE section for disposal of expired acids.

• Rinse previously approved FCA bottles and caps 3 times with Nanopure water. Fill each bottle to approximately the shoulder with Nanopure water and cap the bottle.

• DOC bottles are manufacturer baked amber glass. Fill each bottle with Nanopure water to approximately the shoulder, rinse the cap once with Nanopure water and cap the bottle.

• Place FCA and DOC bottles in fume hood and to each of the bottles designated for the new acid lot, add 1 vial of 4.5N (1:7), 1 mL H2SO4 from the new lot. From an approved acid lot, add 1 vial to each of the designated control samples. Note the acid lots in the NFSS QA logbook.

Labels.) Samples are logged in for analysis by LS2149.

Lot acceptance criteria

• If all data are reported below reporting limits for each sample, the QAS analyst emails SS with approval for sale (see the QASP for email convention details).

• If the data indicate possible contamination with values at or above the reporting limits, a request for verification of rerun information for that data will be made by

QAS to the appropriate group.

o If the data verify below the reporting limits, the QAS analyst emails SS with approval for sale.

o If the data verify at or above the reporting limits, repeat the QA procedure for that (those) constituents.

• If the data indicate sporadic problems for an analyte in the material, then a note will be included on the certificate of analysis that indicates the extent of the problem.

3. Acid, Vial (PP), HCl, 6N, 2 mL Omni Trace

QA procedure, performed by QAS personnel:

• Determine the number of samples to be included in the quality assurance study as directed in the Quality Assurance Surveillance Plan or ask the NFSS QA coordinator.

There are two components to these vials – the acid and the container. If a new lot of vials are to be tested and the acid is of a previously approved acid lot, only 1 new vial is tested with 1 vial from an approved lot. If either the acid or container is of an untested lot, the QA study will typically consist of 9 vials from the new lot and another vial from an approved lot.

• Obtain 3 randomly selected boxes of (24 vials/box) from Support Services (SS).

Also, select 1 vial of acid from a currently approved lot (usually in stock in the QAS laboratory) to be the control sample. Make sure the control lot is not expired.

Contact SHE for disposal of expired acids.

• Rinse previously approved FAM bottles and caps 3 times with Nanopure water. Fill each bottle to about the shoulder with Nanopure water and cap the bottle.

• Place bottles in fume hood and to each of the bottles designated for the new acid lot, add 1 vial of 6N, 2 mL HCl from the new lot. From an approved acid lot, add 1 vial to the designated control sample. Note the acid lots in the NFSS QA logbook.

Labels.) Samples are logged in for analysis by LS2707 (Nutrients).

Lot acceptance criteria:

• If all data are reported below the reporting limits in all the samples, the QAS analyst emails SS with approval for sale (see the QASP for email convention details).

• If the data indicate possible contamination with values at or above the reporting limits, a request for verification of rerun information for that data will be made by

QAS to the appropriate group.

o If the data verify below the reporting limits, the QAS analyst emails SS with approval for sale.

o If the data verify at or above the reporting limits, repeat the QA procedure for that (those) constituents.

• If the data indicate sporatic problems for an analyte in the material, then a note will be included on the certificate of analysis that indicates the extent of the problem.

• If the material is determined to be unacceptable, the QAS NFSS staff will meet with SS personnel to determine the next course of action. This may include returning the material to the vendor.