200.8 Metals Checklist

• Audit Title

• Document No.

• Client / Site

• Conducted on

  Date

• Prepared by

• Location
  Address

• Personnel

Interferences

• Does the data system correct for Isobaric elemental interferences?

  Yes

  No

  N/A

• When memory interferences are noted, is the system flushed with a rinse blank to minimize build-up?

  Yes

  No

  N/A

Sample Collection, etc.

• Has the sample pH been checked; to ensure proper preservation techniques?

  Yes

  No

  N/A

• Sample acidified to <pH2 with nitric acid?

  Yes

  No

  N/A

Reagents and Standards

• Are Ultra High purity reagents used for analysis?

  Yes

  No

  N/A

• D.1.4.b.2 Is the quality of water sources monitored and documented to meet method specified requirements? (ASTM Type I ?)

  Yes

  No

  N/A

• Are fresh multi-element calibration standards prepared every two weeks?

  Yes

  No

  N/A

• Internal Standard

• Is the instrument calibrated by using an internal standard technique?

  Yes

  No

  N/A

• What are the Internal standards? (scandium, yttrium, indium, terbium and bismuth)

  Yes

  No

  N/A

• Are a minimum of three internal standards used (10.3)

  Yes

  No

  N/A

QC

• 5.6.2.b, C.1 Does the laboratory management maintain records to assure that all technical laboratory staff and/or work cells have demonstrated and documented initial and ongoing proficiency in the activities for which they are responsible?

  Yes

  No

  N/A

• Has the upper limit of the linear dynamic range been established?

  Yes

  No

  N/A

• Blanks

• Calibration blank - Consists of 1% (v/v) nitric acid in reagent grade water.

  Yes

  No

  N/A

• Laboratory reagent blank (LRB) - Must contain all the reagents in the same volumes as used in processing the samples. The LRB must be carried through the same entire preparation scheme as the samples including digestion, when applicable.

  Yes

  No

  N/A

• Yes

  No

  N/A

• D.1.1.a Is the method blank processed along with and under the same conditions as the associated samples include all steps of the analytical procedure?

  Yes

  No

  N/A

• Rinse blank - Consists of 2% (v/v) nitric acid in reagent grade water. Rinse blanks should be used to flush the system between blanks, samples, standards and QC samples.

  Yes

  No

  N/A

• Tuning

• D.1.5.c Does the laboratory document acceptance criteria for mass spectral tuning?

  Yes

  No

  N/A

• Tuning solution

  Yes

  No

  N/A

• Be, Mg, Co, In, and Pb; 100 ug/L each in 1% v/v HNO3

  Yes

  No

  N/A

• Prior to analysis each day, does the lab conduct mass calibration and resolution checks using the tuning solution. Resolution at low mass is indicated by magnesium isotopes 24, 25, and 26. Resolution at high mass is indicated by lead isotopes 206, 207, and 208.

  Yes

  No

  N/A

• Is the mass calibration adjusted if it has shifted by more than 0.1 amu from unit mass.

  Yes

  No

  N/A

• Is instrument stability demonstrated by running the tuning solution a minimum of five times with resulting relative standard deviations of absolute signals for all analytes of less than 5%.

  Yes

  No

  N/A

• Laboratory Fortified Blank /LCS & QCS

• Is a QCS analyzed initially and periodically of calibration standards or stock standard solutions in order to verify instrument performance? Is a fresh solution created quarterly or more frequently as needed?

  Yes

  No

  N/A

• D.1.1.b.1 Is a LCS performed at a frequency of 1 per preparation batch of per matrix type, except for analytes for which spiking solutions are not available?

  Yes

  No

  N/A

• The LFB must be carried through the same entire preparation scheme as the samples including sample digestion, when applicable.

  Yes

  No

  N/A

• Are upper and lower control limits for the LFB 85-115%?

  Yes

  No

  N/A

• Is a calibration blank analyzed at the beginning of the run and after each 10 samples, and at the end of the run?

  Yes

  No

  N/A

• Is a calibration check standard analyzed at the beginning of the run and after each 10 samples, and at the end of the run?

  Yes

  No

  N/A

• The analysis of all analytes within the calibration check standard solutions must be within ±10% of calibration.

  Yes

  No

  N/A

• If the calibration cannot be verified within the specified limits, the instrument must be recalibrated.

  Yes

  No

  N/A

• D.1.1.c Does the laboratory document procedures for determining the effect of the sample matrix on method performance? (Matrix Spike) Note: The spiking frequency is 10% of samples.

  Yes

  No

  N/A

• Are the acceptable recovery ranges for the LFM/MS 70-130%?

  Yes

  No

  N/A

• Is the acceptable response for internal standards within 60-125% of the original response of the calibration blank?

  Yes

  No

  N/A

Calibration and Standardization

• At minimum is a blank and a standard used for calibration?

  Yes

  No

  N/A

• 5.9.4.2.1.f If the results of samples are not bracketed by the initial calibration, are the results reported as having less certainty (defined qualifiers, flags, or explanation in the case narrative)?

  Yes

  No

  N/A

• Are 3 integrations averaged for calibration and data reporting?

  Yes

  No

  N/A

• 5.9.4.2.1.d Are all initial calibrations verified with a standard obtained from a second source or lot that is traceable to a national standaed when available? (if the lot can be demonstrated from the manufactureras prepared independently from other lots)

  Yes

  No

  N/A

• 5.9.4.2.1.e Is the criteria for the acceptance of an initial calibration established (QCS standard ± 10% Section 9.2.3)

  Yes

  No

  N/A

• 5.9.4.2.1.g Are corrective actions performed if the results of the initial calibration are outside of established acceptance criteria?

  Yes

  No

  N/A

• 5.9.4.2.1.g Is data associated with unacceptable initial instrument calibration not reported?

  Yes

  No

  N/A

• 5.9.4.2, 5.9.4.2.2 Is a continuing instrument calibration verification used to confirm the continued validity of the initial calibration with each sample batch?

  Yes

  No

  N/A

• Continuing calibration is done after every 10 samples (9.3.4) The results of the CCV are ± 10% for each analyte of interest.

  Yes

  No

  N/A

• If the results are between ±10-15% the previous 10 samples can be used, but the instrument must be recalibrated.

  Yes

  No

  N/A

• If the results are >± 15% the previous 10 samples must be re-analyzed.

  Yes

  No

  N/A

Procedure

• Aqueous Sample Prep – Dissolved Analytes (ground and surface waters)

• Sample volume? (20 mL)

  Yes

  No

  N/A

• Is 0.4 mL of 1:1 HNO3 added to 20 mL of filtered, acid preserved sample? (or equivalent ratio to produce 1% v/v acid/sample) Matrix Matching.

  Yes

  No

  N/A

• Aqueous Sample Prep – Total Recoverable Analytes (drinking water)

• For unfiltered samples < 1 NTU, is the above procedure used?

  Yes

  No

  N/A

• Sample volume? (100 mL)

  Yes

  No

  N/A

• Digestion:

  Yes

  No

  N/A

• -          Add 2mL 1:1 HNO3 and 1mL 1:1 HCl.

  Yes

  No

  N/A

• -          Heat on hot plate at 85C.

  Yes

  No

  N/A

• -          Reduce volume to 20mL.

  Yes

  No

  N/A

• -          Takes 2 hours for reduction. Do not boil sample.

  Yes

  No

  N/A

• -          Cover beaker with watch glass and reflux sample for 30 minutes.

  Yes

  No

  N/A

• -          Cool sample.

  Yes

  No

  N/A

• -          Transfer to 50mL flask, dilute to volume with reagent water.

  Yes

  No

  N/A

• -          Let sit overnight.

  Yes

  No

  N/A

• -          Centrifuge if solids show.

  Yes

  No

  N/A

• -          Adjust chloride concentration.

  Yes

  No

  N/A

• Solid Sample Prep – Total Recoverable Analytes

• Sample weight for percent solids/moisture determination?

  Yes

  No

  N/A

• < 35 % moisture use ~ 20 g

  Yes

  No

  N/A

• > 35 % moisture use ~ 50 – 100 g

  Yes

  No

  N/A

• Is a percent solids calculation used for reporting results on a dry weight basis?

  Yes

  No

  N/A

• Digestion:

  Yes

  No

  N/A

• -          Weigh 1.0 +/- 0.01 g of dried sample

  Yes

  No

  N/A

• -          Add 4 mL 1:1 HNO3 and 10 mL 1:4 HCl.

  Yes

  No

  N/A

• -          Cover with watch glass

  Yes

  No

  N/A

• -          Heat on hot plate at 85C (covered sample refluxes at 95C).

  Yes

  No

  N/A

• -          Reflux for 30 min. Avoid vigorous boiling.

  Yes

  No

  N/A

• -          Cool sample.

  Yes

  No

  N/A

• -          Transfer to 100 mL flask, dilute to volume with reagent water.

  Yes

  No

  N/A

• -          Let sit overnight.

  Yes

  No

  N/A

• -          Centrifuge if solids show.

  Yes

  No

  N/A

• -          Adjust chloride concentration.

  Yes

  No

  N/A

NELAC Related

• D.1.4.a, 5.9.2.a-c Is the source of standards traceable to national standards

  Yes

  No

  N/A

• D.1.6.a Does the laboratory assure that the test instruments consistently operate within the specifications required of the application for which the equipment is used?

  Yes

  No

  N/A

• D.1 Are all quality control measures assessed and evaluated on an on-going basis?

  Yes

  No

  N/A

• D.1 Are the quality control protocols specified by the laboratory’s method manual followed by all analysts?

  Yes

  No

  N/A

• 5.9.4.2.1.b, 5.9.4.2.2.c Are sufficient raw data records retained to permit reconstruction of the initial and continuing calibrations using as appropriate, but not limited to:

  Yes

  No

  N/A

• a.___ Calibration date

  Yes

  No

  N/A

• b.___ Test method

  Yes

  No

  N/A

• c.___ Instrument

  Yes

  No

  N/A

• d.___ Analysis date

  Yes

  No

  N/A

• e.___ Each analyte name

  Yes

  No

  N/A

• f.___ Analyst's initials or signature

  Yes

  No

  N/A

• g.___ Concentration and response

  Yes

  No

  N/A

• h.___ Response

  Yes

  No

  N/A

• i.___ Calibration curve or response factor, or

  Yes

  No

  N/A

• j.___ Unique equation or coefficient used to reduce instrument responses to concentration.

  Yes

  No

  N/A

• 5.9.4.1.d Prior to use on each working day, are balances, ovens, refrigerators, freezers, incubators and water baths checked with NIST traceable references (where available) in the expected use range?

  Yes

  No

  N/A

• 5.9.2.a Are measurements made by the labs traceable to national standards of measurement where available?

  Yes

  No

  N/A

• 5.10.5.a Does the laboratory retain records for all standards, reagents and media including manufacturer/vendor, the manufacturer’s Certificate of Analysis or purity (if supplied), date of receipt, recommended storage conditions, and an expiration date after which the material shall not be used unless its reliability is verified by the laboratory?

  Yes

  No

  N/A

• 5.9.4.1.c Are all raw data records retained to document equipment performance? (i.e. maintenance logs)

  Yes

  No

  N/A

• 5.9.4.1.e Are mechanical volumetric devices, including burettes, checked for accuracy on at least a quarterly use basis?

  Yes

  No

  N/A

• 2.5 Do the laboratory's management and all analysts ensure that all PT samples are handled (i.e., managed, analyzed, and reported) in the same manner as real environmental samples utilizing the same staff, methods as used for routine analysis of that analyte, procedures, equipment, facilities, and frequency of analysis?

  Yes

  No

  N/A

• Assessor

  Sign

• Lab Representative

  Sign