TNI Logo The NELAC Institute

TNI Standards Guidance

Disclaimer: This material represents the opinion of its authors. It is intended solely as guidance and does not include any mandatory requirements except where such requirements are referenced. This guidance does not establish expectations of being implemented universally, exclusively, in whole, or in part.

This guidance does not establish or affect legal rights or obligations and is not finally determinative of the issues it addresses. It does not create any rights enforceable by any party in litigation with TNI, its accreditation bodies, or affiliated institutions. Any decisions made by TNI regarding requirements addressed in this guidance will be made by applying the applicable standards, policies or procedures to the relevant facts.

 

Module: Quality Systems


Subject: Extent of Analytical Records

Question 1

How much information is required to be tied to analytical records?  For instance, if a reagent used for part of an analysis requires it to be dried prior to weighing, do you really have to record the particular oven used, balance used, time/temp in oven and time/temp out of oven and reference these records in your final analytical record for analysis?

The lot or tracking number of each specific reagent must be noted with the analytical records, but if the specific details regarding the preparation of the reagent is included in a laboratory SOP, that should generally be sufficient to comply with the requirement in this section of the TNI Standard; however additional documentation may be necessary where steps are considered integral to the analytical process and where the lack of specific information could jeopardize the validity of the test method performance. 

Where clear direction for mandatory conditions are present in the published method for the analysis of a parameter (i.e. incubation times/temperatures, digestion times/temperature, drying times/temperature, etc.); then sufficient documentation must be present to allow for the clear demonstration that the condition have been met during field sample analysis.  As in the case of TCLP leaching of field samples using EPA 1311, the conditions of the tumbling environment must be documented to demonstrate that the field sample leaching was compliant with the method requirements (i.e. tumbled at 30 + 2 rpm for 18 + 2 hours in ambient temperature 23 ­+ 2°C.  These are critical conditions to the quality of the leachate being extracted from the field samples.  Leaching performed with a rotation that does not meet method requirements may not sufficiently agitate to extract the target analytes from the sample matrices as would be the case if samples are leached for less time.  If the temperature of the leaching environment is higher than 25°C, then more volatile target analytes may dissipate from the leachate and be lost producing false negatives in the test results.  The documentation and the ability to demonstrate the conditions in this example are critical to the method performance and will affect the validity of the test performance.  Another example would be the documentation of the conditions of sample digestion for metallic analytes by ICP or ICPMS.  The hotplate temperature must be 95°C + 5°C and this must be clearly documented during sample preparation to demonstrate that a complete digestion occurred. 

In other areas, conditions that are not critical can typically be documented in an SOP, but specific demonstrations are not required for each item.  This is the case with reagents where drying must occur for 4 hours, as is the case with sodium sulfate used in the extractions of organic samples.  The drying of sodium sulfate is required at 400°C for 4 hours, as specified by EPA 3510C.  Whether the sodium sulfate is dried for 4 hours or allowed to dry for 8 hours is not imperative.  What is imperative in this requirement is that sufficient dryness occurs to allow the sodium sulfate to absorb the moisture that may be present in solvents used during sample extraction.  The time frame for the drying process is not a critical step as long as the 4 hour minimum is achieved.  The conditions used for drying this product can be documented in SOP form and daily documentation is not required.            



References:

NELAC 2003 Section 5.4.12.2.5.3

Analytical Records

The essential information to be associated with analysis, such as strip charts, tabular printouts, computer data files, analytical notebooks, and run logs, shall include:

  1. laboratory sample ID code;
  2. date of analysis and time of analysis is required if the holding time is 72 hours of less or when time critical steps are included in the analysis, e.g., extractions, and incubations;
  3. Instrumentation identification and instrument operating conditions/parameters (or reference to such data);
  4. analysis type;
  5. all manual calculations, e.g., manual integrations; and,
  6. analyst’s or operator’s initials/signature;
  7. sample preparation, including cleanup, separation protocols, incubation periods or subculture, ID codes, volumes, weights, instrument printouts, meter readings, calculations, reagents;
  8. sample analysis;
  9. standard and reagent origin, receipt, preparation, and use;
  10. calibration criteria, frequency and acceptance criteria;
  11. data and statistical calculations, review, confirmation, interpretation, assessment and reporting conventions;;
  12. quality control protocols and assessment;
  13. electronic data security, software documentation and verification, software and hardware audits, backups, and records of any changes to automated data entries;
  14. method performance criteria including expected quality control requirements.

 

2009 TNI V1M2 4.13.3 f

4.13.3 Additional Requirements
f)     All information necessary for the historical reconstruction of data shall be maintained by the laboratory.

  1. all raw data, whether hard copy or electronic, for calibrations, samples and quality control measures, including analysts’ worksheets and data output records (chromatograms, strip charts, and other instrument response readout records);
  2. a written description or reference to the specific method used, which includes a description of the specific computational steps used to translate parametric observations into a reportable analytical value;
  3. laboratory sample ID code;
  4. date of analysis;
  5. time of analysis is required if the holding time is seventy-two (72) hours or less, or when time critical steps are included in the analysis (e.g., extractions and incubations);
  6. instrumentation identification and instrument operating conditions/parameters (or reference to such data);
  7. all manual calculations;
  8. analyst's or operator's initials/signature or electronic identification;
  9. sample preparation, including cleanup, separation protocols, incubation periods or subculture, ID codes, volumes, weights, instrument printouts, meter readings, calculations, reagents;
  10. test results;
  11. standard and reagent origin, receipt, preparation, and use;
  12. calibration criteria, frequency and acceptance criteria;
  13. data and statistical calculations, review, confirmation, interpretation, assessment and reporting conventions;
  14. quality control protocols and assessment;
  15. electronic data security, software documentation and verification, software and hardware audits, backups, and records of any changes to automated data entries;
  16. method performance criteria including expected quality control requirements;
  17. proficiency test results;
  18. records of demonstration of capability for each analyst; and
  19. a record of names, initials, and signatures for all individuals who are responsible for signing or initialing any laboratory record.