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HomeMy WebLinkAbout#591_9_2014_REVISED_Final INSPECTION REPORT ROUTING SHEET To be attached to all inspection reports in-house only. Laboratory Cert. #: 591 Laboratory Name: Environmental Conservation Laboratories, Inc. Inspection Type: Commercial Maintenance Inspector Name(s): Nick Jones, Dana Satterwhite, Gary Francies, Todd Crawford, Tonja Springer, Jason Smith and Beth Swanson Inspection Date: September 9th and 10th, 2014 Date Report Completed: October 9, 2014 Date Forwarded to Reviewer: October 9, 2014 Reviewed by: Todd Crawford Date Review Completed: October 16, 2014 Cover Letter to use: Insp. Initial Insp. Reg. Insp. No Finding Insp. CP Corrected Unit Supervisor/Chemist III: Gary Francies Date Received: 10/16/2014 Date Forwarded to Linda: 11/18/2014 Date Mailed: 11/18/2014 cc: Carrie Ruhlman Chris Goforth On-Site Inspection Report LABORATORY NAME: Environmental Conservation Laboratories, Inc. ADDRESS: 102 Woodwinds Industrial Ct. Ste. A Cary, NC 27511-6204 CERTIFICATE #: 591 DATE OF INSPECTION: September 9th and 10th, 2014 TYPE OF INSPECTION: Commercial Maintenance AUDITOR(S): Nick Jones, Dana Satterwhite, Gary Francies, Todd Crawford, Tonja Springer, Jason Smith and Beth Swanson LOCAL PERSON(S) CONTACTED: Dale Mori, Lori Mangrum, Rich Detar I. INTRODUCTION: This laboratory was inspected by representatives of the North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC) program to verify its compliance with the requirements of 15A NCAC 2H .0800 for the analysis of environmental samples. II. GENERAL COMMENTS: The laboratory was clean and well organized. The facility has all the equipment necessary to perform the analyses. The system for traceability of standard and reagent preparation is effective, thorough and easy to follow. Laboratory personnel communicate well and coordinate sample analyses effectively to manage workload and holding times. Proficiency Testing (PT) samples have been analyzed for all certified parameters for the 2014 proficiency testing calendar year and the graded results were 100% acceptable. The laboratory is reminded that any time changes are made to laboratory operations; the laboratory must update the Quality Assurance (QA)/Standard Operating Procedures (SOP) document(s). Any changes made in response to the Findings, Recommendations or Comments listed in this report must be incorporated to insure the method is being performed as stated, references to methods are accurate, and the QA and/or SOP document(s) is in agreement with approved practice and regulatory requirements. In some instances, the laboratory may need to create a SOP to document how new functions or policy will be implemented. Contracted analyses are performed by Environmental Conservation Laboratories, Inc. (Certification #s 424 and 442). Page 2 #591 – Environmental Conservation Laboratories, Inc. Current quality assurance policies for both Field and Non-Field Laboratories and approved procedures for the analysis of the facility’s currently certified Field parameters were provided at the time of the inspection. The requirements associated with Findings A, C, M, N, S, and U have been implemented by our program since the last inspection. III. FINDINGS, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS: General Laboratory A. Finding: The temperature corrections for the laboratory thermometers are not being posted when they are zero. Requirement: All thermometers and temperature measuring devices must be checked every 12 months against a NIST certified or NIST traceable thermometer and the process documented. To check a thermometer or the temperature sensor of a meter, read the temperature of the thermometer/meter against a NIST certified or NIST traceable thermometer and record the two temperatures. The calibration must be performed at a temperature that corresponds to the temperature used by the incubator, refrigerator, freezer, etc. In the case of temperature measuring devices used to perform variable temperature readings the calibration must be performed at a temperature range that approximates the range of the samples. The thermometer/meter readings must be less than or equal to 1ºC from the NIST certified or NIST traceable thermometer reading. The documentation must include the serial number of the NIST certified thermometer or NIST traceable thermometer that was used in the comparison. Also make any corrections to the data and document any correction that applies (even if zero) on both the thermometer/meter and on a separate sheet to be filed. Ref: NC WW/GW LC Policy. Quality Control B. Finding: The Laboratory Information Management System (LIMS) reports an incorrect dilution factor on the Quality Control Data Report for spiked samples when that sample also has to be diluted. This is considered pertinent information. Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A). Comment: This was observed on an Ammonia (as N) sample (C401639); however, since this appears to be a LIMS limitation, it may actually be a laboratory-wide issue. In this particular instance, the sample was spiked and diluted 100x, but the dilution factor (DF) was incorrectly reported as 1 on the Quality Control Data Report. The practical quantitation limit (PQL) was adjusted for the 100x dilution appropriately. Recommendation: If the LIMS cannot be programmed to properly report the dilution factor for matrix spike samples that must be diluted, it is recommended that a data flag or remark code be used to document the proper dilution factor on the Quality Control Data Report. Page 3 #591 – Environmental Conservation Laboratories, Inc. C. Finding: Error corrections on data are not always performed properly. Requirement: All documentation errors must be corrected by drawing a single line through the error so that the original entry remains legible. Entries shall not be obliterated by erasures or markings. Wite-Out®, correction tape or similar products designed to obliterate documentation are not to be used. Write the correction adjacent to the error. The correction must be initialed by the responsible individual and the date of change documented. All data and log entries must be written in indelible ink. Pencil entries are not acceptable. Ref: North Carolina Wastewater/ Groundwater Laboratory Certification Policy. Comment: Error corrections are usually initialed by the analyst making the correction, but the date of change is not always documented. Comment: Observed on Sulfide sample (4D23013). Recommendation: It is recommended that when any documentation correction that affects the final reported sample result is made, the lab also note the reason the change was made. For example, changing an original sample absorbance or weight observation due to further stabilization of the spectrophotometer or balance, the lid to the spectrophotometer was left open in error during sample measurement, etc. Documentation Recommendation: The benchsheets and/or preparatory sheets for several parameters contained a column with a header for units which commonly read “mL / g.” The analyst was expected to circle one or the other as appropriate to the analysis. Often times neither unit of measure was circled. Additionally, the spaces below the header were often used for dilution factors. It is recommended the column be modified so that its intended use would be intuitive. Splitting the header horizontally; moving its current contents to the top half; and inserting Dilution or DIL in the bottom half would be a simple, satisfactory solution. Recommendation: It is recommended that Standard Operating Procedures include a revision history with relevant dates and a brief description of the change(s) made. D. Finding: An inconsistency was noted between the Standard Operating Procedure (SOP) and laboratory practice as follows: • During the SOP review process, all current methods are to be compared to the most recent 40 CFR Part 136 Methods Update Rule (MUR), published on May 18, 2012, to ensure the most recently approved method version is being used and that all benchsheets are updated to accurately reflect those references and current protocol. • The method reference in the SOP is not correct (this does not necessarily refer to each SOP’s primary reference, but may refer to minor references found in the bodies of the SOPs). o Settleable Solids – remove all reference to EPA Method 160.5. Page 4 #591 – Environmental Conservation Laboratories, Inc. o Nitrite (as N) – update reference in section 4.2. o Orthophosphate – update reference in section 4.4. o Ammonia (as N) – missing revision number and year. o Cyanide – missing reference year. • Personnel were not following procedures as stated in the laboratory’s SOP. o Total Kjeldahl Nitrogen (TKN) – Table 4 in the SOP lists the blank acceptance criterion as “<½MRL”; however, the criterion used is “<MRL.” NC WW/GW LC policy requires: For analyses requiring a calibration curve, the concentration of reagent, method and calibration blanks must not exceed 50% of the reporting limit (i.e., ≤½MRL) or as otherwise specified by the reference method. • The SOP does not describe in sufficient detail how the method is performed. o The matrix spike (MS) /matrix spike duplicate (MSD) preparation and/ or calculations are not adequately described.  Mercury – both matrices  Hexavalent Chromium  Ion Chromatography (IC)  Orthophosphate  Chloride  MBAS  Chemical Oxygen Demand  Phosphorus, Total  Organics Comment: When correcting the above-stated documentation issues in the SOPs regarding the MS/MSD preparation and/or calculation, ensure that the spike to sample volume ratio requirement in the NC WW/GW Matrix Spiking Policy 05/11/2012 is met. A copy of this policy is attached to this report. o Fecal Coliform – Section 11.1 needs clarification of preservation and storage of samples (i.e., actual temperature during storage). o SEAL AQ2 – For all parameters analyzed using the SEAL AQ2 discrete analyzer, include the instrument software equations used to calculate environmental and quality control sample results so that calculated data results can be reconstructed. o Total Kjeldahl Nitrogen (TKN) – The acid used to reduce pH to ≤ 2 is not identified (i.e., H2SO4). Page 5 #591 – Environmental Conservation Laboratories, Inc. o Total Dissolved Solids (TDS) – Section 14.17 states that the sample is to be transferred to a 180°C oven for at least an hour after evaporation. Clarification of the drying procedure after evaporation is needed (i.e. desiccation and constant weight). o The word “should” is utilized in many SOPs. Standard Operating Procedures must reflect what is actually being done in the laboratory. • The following SOPs specify the blank acceptance criterion as <MRL; must be ≤ ½ MRL. o Ammonia (as N) o Nitrite (as N) – SM 4500-NO3 F-2000 and EPA 353.2, Rev. 2.0 (1993) o Nitrate+Nitrite (as N) – SM 4500-NO3 F-2000 and EPA 353.2, Rev. 2.0 (1993) o Ion Chromatography o Orthophosphate – SM 4500 P F-1999 and EPA 365.1, Rev. 2.0, 1993 o Chloride – SM 4500 Cl E-1997 o Cyanide o MBAS o Chemical Oxygen Demand o Alkalinity – EPA Method 310.2 o Mercury – both matrices o All Organics o Metals – Inductively Coupled Plasma-Atomic Emission Spectrometer and Inductively Coupled Plasma-Mass Spectrometer Comment: SOP# QAQC-32 states in Figure 2 that results are qualified only if “Result <5xMRL (organics) or <2xMRL (inorganics).” • The SOP contains language not found in, or contradictory to, the method. o Biochemical Oxygen Demand (BOD) – Section 6.4 reads: “The maximum time between start of processing of the first and last sample in the batch is 24 hours.” Seed material must be used within 6 hours after preparation per the manufacturer’s instructions. o Carbonaceous Biochemical Oxygen Demand (CBOD) - Sections 12.1 and 14.2.6 state that nitrification inhibitor is being added to the blank. The method [i.e., SM 5210 B-2001 (6) (c)] explicitly states that nitrification inhibitor must not be added to the blank. o BOD/CBOD - Section 14.3.2.1 states initial D.O. must be between 7.0 – 9.0 mg/L. The method [i.e., SM 5210 B-2001 (5) (a)] specifies that initial DO must be between 7.5 – 9.0 mg/L. o BOD/CBOD - Section 9.8 states that indicator strips are used to prescreen for the presence/ absence of total residual chlorine. DPD powder must be used unless the sample contains interferences for DPD powder per NC WW/GW LC Policy. Page 6 #591 – Environmental Conservation Laboratories, Inc. o TKN – Section 11.2 states samples are preserved to “pH ≤ 2”. The Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, May 18, 2012, Table II requires “pH <2”. • The SOP does not describe the procedure/calculation to be used when the weight gain requirement is not met and less than 1000 ml of sample is analyzed for the following parameters. o Total Suspended Residue o Total Dissolved Residue o Total Residue Comment: See the attached NC WW/GW residue policies for guidance. • Color, Platinum Cobalt (PtCo) – The SOP does not state the frequency in which a new calibration curve is prepared/ analyzed. • Color, Platinum Cobalt (PtCo) – The SOP does not describe adjustment of pH, when necessary. • Nitrate+Nitrite (as N) – The laboratory control standard acceptance criterion is stated as ±20% in the SOP. EPA Method 353.2 [Section 9.3.2] requires ±10% for the laboratory control standard (referred to as a laboratory fortified blank in the method) acceptance criterion. • Nitrate+Nitrite (as N) and MBAS – A naming inconsistency was noticed. The SOPs refer to a laboratory control standard. The preparation log and/or benchsheet refer to a blank spike. • TKN and Ammonia (as N) – Specify the type of regression equation used to calculate results. • TKN and Ammonia (as N) - Regarding sample preservation, the SOPs state “…cooling to ≤6 °C …” This needs to be modified to state “…cooling to ≤6 °C without evidence of freezing” to match footnote 18 of Table II in the Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, May 18, 2012. • Metals Inductively Coupled Plasma-Mass Spectrometer – The mathematic symbol “≥” needs to be added to the values for the acceptable curve correlation coefficient in Table 7. Requirement: Each laboratory shall develop and maintain a document outlining the analytical quality control practices used for the parameters included in their certification. Supporting records shall be maintained as evidence that these practices are being effectively carried out. Ref: 15A NCAC 2H .0805 (a) (7). Requirement: The laboratory must have an updated Quality Control/Standard Operating Procedures document for the parameters included on the certificate attachment. Please submit all SOPs that have been revised in response to this inspection by June 1, 2015. A written response is required. Page 7 #591 – Environmental Conservation Laboratories, Inc. Recommendation: BOD - Section 16.5 states an acceptance criterion of ±20% on the Winkler titration verification. This can be a relatively large concentration. Instead of expressing the criterion as a percentage, it is recommended that it be expressed as a concentration (e.g., ±0.5 mg/L). Recommendation: Cyanide – Section 11 states preservation to pH ≥ 12. It is recommended that this be changed to pH > 10 to match the requirement found in Table II in the Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, May 18, 2012. Alkalinity – EPA Method 310.2 (Rev. 1974) Recommendation: Change reporting units from micrograms per liter to milligrams per liter. E. Finding: The laboratory filters turbid samples prior to analysis by EPA Method 310.2, Rev. 1974. Requirement: Sample turbidity and color may interfere with this method. Turbidity must be removed by filtration prior to analysis. If sample is filtered, this method is not approved for NPDES monitoring. Sample color that absorbs in the photometric range used will also interfere. Ref: EPA Method 310.2, Rev. 1974, Section 4.1. Comment: All NPDES samples which would normally have to be filtered to be analyzed by EPA Method 310.2, Rev. 1974 must be analyzed by SM 2320 B- 1997 (titration). Note: Filtration is not allowed for titrimetric analysis either. It is acceptable to analyze non-NPDES samples by EPA Method 310.2, Rev. 1974. This data must be clearly labeled as non-NPDES data. Recommendation: It is recommended that no samples be filtered and analyzed by EPA Method 310.2, Rev. 1974. F. Finding: The lab is analyzing the calibration standards in order of increasing concentration. Requirement: Place working standards in sampler in order of decreasing concentration. Ref: EPA Method 310.2 (Rev. 1974), Section 7.4. Specific Conductance – Standard Methods, 2510 B-1997 G. Finding: The Automatic Temperature Compensator (ATC) has not been verified. Cited Previously on 12/7/2007. Requirement: The ATC must be verified annually (i.e., every twelve months) and the process documented. The ATC must be verified by analyzing a standard at 25 °C (the temperature that conductivity values are compensated to) and a temperature(s) that brackets the temperature ranges of the samples to be Page 8 #591 – Environmental Conservation Laboratories, Inc. analyzed. This may require the analysis of a third temperature reading that is > 25 °C. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy. Comment: The NC WW/GW LC Approved Procedure for the Analysis of Specific Conductance (Conductivity) has been attached for guidance regarding the verification procedure of the ATC. Color, Platinum Cobalt (PtCo) – Standard Methods, 2120 B-2001 Recommendation: It is recommended that the date and time of sample collection be documented on the benchsheets. H. Finding: The unit of measure (e.g., S.U.) for the sample pH column is not documented on the benchsheets. Requirement: All laboratories must use printed laboratory bench worksheets that include a space to enter the signature or initials of the analyst, date of analyses, sample identification, volume of sample analyzed, value from the measurement system, factor and final value to be reported and each item must be recorded each time samples are analyzed. The date and time BOD and coliform samples are removed from the incubator must be included on the laboratory worksheet. Ref: 15A NCAC 2H .0805 (a) (7) (H). pH – Standard Methods, 4500 H+ B-2000 Comment: Duplicate analyses are no longer required for field parameters. Comment: The lab’s established check buffer acceptance criterion for the 7.0 buffer is ± 0.1%, which is 6.93 - 7.07 S.U. The lab could use ± 0.1 S.U. [per SM 4500 H+ B-2000 (4) (a)] as the acceptance criterion. I. Finding: The benchsheets reference EPA Method 150.1, a method no longer approved for NPDES compliance monitoring. Requirement: The approved Clean Water Act (CWA) Method is SM 4500 H B- 2000. Ref: Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, May 18, 2012. Comment: The lab was not certified for or reporting results by EPA Method 150.1. Solids, Total Dissolved – Standard Methods, 2540 C-1997 Solids, Total Suspended – Standard Methods, 2450 D-1997 Solids, Total – Standard Methods, 2540 B-1997 J. Finding: The laboratory is reporting data below the reporting limit as established by the method. Requirement: The minimum reporting value is established at 2.5 mg/L when 1000 mL of sample is analyzed. The minimum weight gain allowed by any approved method is 2.5 mg. In instances where the weight gain is less than the Page 9 #591 – Environmental Conservation Laboratories, Inc. required 2.5 mg, the value must be reported as less than the appropriate value based upon the volume used. For example, if 500 mL of sample is analyzed and < 2.5 mg of dried residue is obtained, the value reported would be < 5 mg/L. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy. Requirement: Choose sample volume to yield between 2.5 and 200 mg dried residue. To obtain the required residue yield, successive aliquots of samples may be added to the same dish after evaporation or adjust reporting level based upon the weight gain and sample volume used. For example, if 100 mL sample is analyzed, and less than 2.5 mg of dried residue is obtained, the value reported would be <25 mg/L. The minimum reporting value is established at 2.5 mg/L based upon a sample volume used of 1000 mL. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy. Comment: The PQL is not adjusted for sample volume in the Laboratory Information Management System (LIMS) causing the lab to sometimes report analytical results below the reporting limit for the sample volume used. BOD/CBOD – Standard Methods, 5210 B-2001 Comment: Seed correction factors outside of 0.6-1.0 mg/L no longer have to be qualified. Recommendation: Analyze a seeded blank with each sample batch. The value should approximate (i.e., ~ ±0.2 mg/L) the calculated seed correction factor (SCF) and will provide useful information about analyst technique and homogeneity of seed material. K. Finding: The lab is utilizing indicator strips to verify the presence/absence of residual chlorine. Requirement: It is acceptable to screen samples with DPD powder for the presence of total residual chlorine (use pillows appropriate for the volume of sample tested). Generally, total residual chlorine test strips are not adequate; however, these may be used for samples where interference with DPD precludes their use. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy. L. Finding: Data that does not meet all quality control requirements is not qualified on the client report. Requirement: When quality control (QC) failures occur, the laboratory must attempt to determine the source of the problem and must apply corrective action. Part of the corrective action is notification to the end user. If data qualifiers are used to qualify samples not meeting QC requirements, the data may not be useable for the intended purposes. It is the responsibility of the laboratory to provide the client or end-user of the data with sufficient information to determine the usability of the qualified data. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy. Page 10 #591 – Environmental Conservation Laboratories, Inc. Recommendation: BOD – Update the B-03 Flag in the LIMS to <0.20 mg/L. It is currently <0.2 mg/L. The second decimal place is required per SM 5210B-2001 (6) (c). M. Finding: Extra nutrient, mineral, and buffer solutions are not added to the Biochemical Oxygen Demand (BOD) bottles containing more than 67% (i.e., > 201 mL) sample. Requirement: When a bottle contains more than 67% of the sample after dilution, nutrients may be limited in the diluted sample and, subsequently, reduce biological activity. In such samples, add the nutrient, mineral, and buffer solutions (3a through e) directly to individual BOD bottles at a rate of 1 mL/L (0.30 mL/300-mL bottle) or use commercially-prepared solutions designed to dose the appropriate bottle size. Ref: Standard Methods, 5210 B-2001, (5) (c) (2). Comment: Dilution water prepared as normal with nutrient, mineral, and buffer solutions would still be used in the BOD bottles. For the bottles containing more than 67% sample, extra nutrient, mineral, and buffer solutions would be added in addition to the dilution water. Recommendation: Rather than pipetting 0.30 mL of each reagent into the BOD bottle, it is recommended that commercially prepared nutrient buffer pillows for 300 mL bottles be used. N. Finding: The lab is performing dilutions greater than 1:100 utilizing micro-pipettes. Requirement: Sample volumes less than 20 mls must be measured using a wide-tip pipet. For dilutions greater than 1:100 make a primary dilution before making final dilution. This would be any measurements of less than 3 mls sample volume if diluting directly into BOD bottles. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy. Comment: Micro-pipettes are not to be used for measuring samples for BOD analysis. Sulfide – Standard Methods, 4500 S2- D-2000 Recommendation: Document the cell path length used on the laboratory benchsheets. O. Finding: The lab does not analyze a filtered blank and standard when samples are filtered due to turbidity after the additions of reagents 1 and 2. Requirement: Minimum Quality Control requirements include a method blank and a laboratory fortified blank. Ref: Standard Methods, Table 4020:I. Requirement: A reagent blank (method blank) consists of reagent water (see Section1080) and all reagents (including preservatives) that normally are in contact with a sample during the entire analytical procedure. The reagent blank is used to determine whether and how much reagents and the preparative Page 11 #591 – Environmental Conservation Laboratories, Inc. analytical steps contribute to measurement uncertainty. Ref: Standard Methods, 1020 B-2011 (5). Requirement: A laboratory-fortified blank [laboratory control standard (LCS)] is a reagent water sample (with associated preservatives) to which a known concentration of the analyte(s) of interest has been added...Process the LFB through all sample preparation and analysis steps. Ref: Standard Methods, 1020 B-2011 (6). Orthophosphate – EPA Method 300.0, Rev. 2.1 (1993) Orthophosphate – EPA Method 365.1, Rev. 2.0 (1993) Orthophosphate – Standard Methods, 4500 P F-1999 Orthophosphate – SW-846 Method 9056 A P. Finding: The samples are not filtered in the field and/or the filtration is not documented. Requirement: Filter within 15 minutes. Ref: Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, May 18, 2012; Table II. Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A). Comment: Upon arrival at the lab the Orthophosphate samples often share a sample bottle with other parameters precluding filtration in the field. Comment: A notation of time filtered on the Chain of Custody would verify whether the samples are compliant upon arrival at the lab. Recommendation: It is recommended that the lab communicate with sample collectors to ensure they are aware of the requirements regarding sample filtration. Ammonia Nitrogen – EPA Method 350.1, Rev. 2.0 (1993) Total Kjeldahl Nitrogen – EPA Method 351.2, Rev. 2.0 (1993) Q. Finding: The laboratory is not analyzing a Laboratory Fortified Matrix at a minimum frequency of 10% of routine samples. Requirement: The laboratory must add a known amount of analyte to a minimum of 10% of the routine samples. Ref: EPA Method 350.1, Rev. 2.0 (1993), Section 9.4.1. Requirement: The laboratory must add a known amount of analyte to a minimum of 10% of the routine samples. Ref: EPA Method 351.2, Rev. 2.0 (1993), Section 9.4.1. Comment: The laboratory is analyzing a Laboratory Fortified Matrix sample at a frequency of 5% of routine samples. Nitrate+Nitrite (as N) – EPA Method 353.2, Rev. 2.0 (1993) Page 12 #591 – Environmental Conservation Laboratories, Inc. Nitrate+Nitrite (as N) – Standard Methods, 4500 NO3ˉ F-2000 Nitrite (as N) – EPA Method 353.2, Rev. 2.0 (1993) Nitrite (as N) – Standard Methods, 4500 NO3ˉ F-2000 Nitrate (as N) – [NO2 + NO3 EPA Method 353.2, Rev. 2.0 (1993)] – [NO2 EPA Method 353.2, Rev. 2.0 (1993)] Nitrate (as N) – (NO2 + NO3 Standard Methods, 4500 NO3ˉ F-2000) - (NO2 Standard Methods, 4500 NO3ˉ F-2000) R. Finding: The lab is not certified for methods which are referenced on the Nitrogen calculation sheet. • Referenced Standard Methods, 4500 NO3ˉ H for Nitrate Nitrogen. • Referenced Standard Methods, 4500 NO2ˉ B for Nitrite Nitrogen. • Referenced EPA Method 354.1 for NO2+NO3 Nitrogen. It is also not an approved method per 40 CFR Part 136. Requirement: Commercial laboratories are required to obtain certification for parameters which will be reported by the client to comply with State surface water monitoring, groundwater, and pretreatment Rules. Ref: 15A NCAC 02H .0804 (a). Chloride – EPA Method 300.0, Rev. 2.1 (1993) Chloride – SW-846 Method 9056 A COD – EPA Method 410.4, Rev. 2.0 (1993) COD – Standard Methods, 5220 D-1997 Fluoride – EPA Method 300.0, Rev. 2.1 (1993) Fluoride – SW-846 Method 9056 A Nitrate+Nitrite (as N) – EPA Method 300.0, Rev. 2.1 (1993) Nitrate+Nitrite (as N) – SW-846 Method 9056 A Nitrate (as N) – EPA Method 300.0, Rev. 2.1 (1993) Nitrate (as N) – SW-846 Method 9056 A Nitrite (as N) – EPA Method 300.0, Rev. 2.1 (1993) Nitrite (as N) – SW-846 Method 9056 A Orthophosphate – EPA Method 300.0, Rev. 2.1 (1993) Orthophosphate – SW-846 Method 9056 A Sulfate – EPA Method 300.0, Rev. 2.1 (1993) Sulfate – SW-846 Method 9056 A Mercury – EPA Method 245.1, Rev. 3.0 (1994) Mercury – SW-846 Method 7470 A Mercury – SW-846 Method 7471 B S. Finding: The laboratory is exceeding 1% sample volume with spiking solution when preparing matrix spikes and is not using the proper correction factor when calculating the final result. Requirement: The volume of spike solution used in matrix spike preparation must in all cases be ≤ 10% of the total matrix spike volume. It is preferable that the spike solution constitutes ≤ 1% of the total matrix spike volume so that the matrix spike can be considered a whole volume sample with no adjustment by calculation necessary. If the spike solution volume constitutes >1% of the total sample volume, the sample concentration or spike concentration must be Page 13 #591 – Environmental Conservation Laboratories, Inc. adjusted by calculation. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy. Mercury – EPA Method 245.1, Rev. 3.0 (1994) Mercury – SW-846 Method 7470 A Mercury – SW-846 Method 7471 B Comment: There was a trend of negative blank values. Recommendation: It is recommended that an acceptance criterion for negative blank values be established. EPA Region IV recently stated in a meeting that up to half the reporting limit concentration on the negative side was acceptable. Recommendation: It is recommended the laboratory determine the root cause of the negative blank values and take steps to optimize the system to prevent persistent recurrence. Hexavalent Chromium – Standard Methods 3500-Cr B-2009 T. Finding: Non-LIMS generated benchsheets do not document sample preparation (reagent addition), time, reaction time, or analysis time. This is considered pertinent information. Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A). Comment: Due to the short hold time, the analysts analyze the samples before the LIMS benchsheet can be generated. 1,2-Dibromoethane (EDB) – EPA Method 504.1 1,2-Dibromoethane (EDB) – SW-846 Method 8011 Comment: The laboratory has not analyzed any samples by EPA Method 504.1. EPA Method 504.1 is the designated method for ethylene dibromide in groundwater samples. The laboratory reports ethylene dibromide by SW-846 Method 8260 B. Please note that other EPA-approved analytical methods may be used if the methods include the same constituents as the analytical methods specified and meet the detection limits of the analytical methods. U. Finding: Manual integration was being used as a substitute for instrument optimization and maintenance on the chromatographic system. Requirement: Under no circumstances will manual integration be performed solely for the purpose of meeting quality control criteria, nor is it to be used as a substitute for proper sample preparation (e.g., cleanup), proper instrument optimization or maintenance on the chromatographic system. Corrective actions, with regard to the instrumentation for computer software, must be taken if manual integrations become common for an analysis or an instrument that normally uses automated peak integration. Ref: North Carolina Wastewater/Groundwater Laboratory Certification Policy. Page 14 #591 – Environmental Conservation Laboratories, Inc. Field Parameters Comment: Standard Operating Procedures (SOPs) had not been developed for all of the parameters included on the laboratory’s certificate attachment (i.e., field parameters pH and Temperature).The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) states: Each laboratory shall develop and maintain a document outlining the analytical quality control practices used for the parameters included in their certification. Supporting records shall be maintained as evidence that these practices are being effectively carried out. Demonstration of acceptable corrective action (i.e., a Field Parameter Standard Operating Procedure) was received by email on 10/30/2014. No further response is necessary for this finding. V. Finding: Temperature - The laboratory is analyzing samples and reporting data for parameters without North Carolina Wastewater/Groundwater Laboratory Certification. Requirement: Commercial laboratories are required to obtain certification for parameters which will be reported by the client to comply with State surface water monitoring, groundwater, and pretreatment Rules. Ref: 15A NCAC 02H .0804 (a). Comment: The laboratory submitted an application amendment form to add Temperature to their certificate on October 7, 2014. An additional parameter invoice (# 023429) was sent to the lab on October 27, 2014. The lab submitted an SOP on October 30, 2014. W. Finding: pH - The field benchsheet does not document: Time of sample collection/analysis; instrument ID; or pH units (i.e., S.U.). This is considered pertinent information. Requirement: All analytical data pertinent to each certified analysis must be filed in an orderly manner so as to be readily available for inspection upon request. Ref: 15A NCAC 2H .0805 (a) (7) (A). IV. PAPER TRAIL INVESTIGATION: The paper trail consisted of comparing laboratory chain of custodies, laboratory benchsheets and client reports. Data were reviewed for the following project numbers: • BOD 3/26/2014 – C403900-01, C403900-02 • Residue, Total Suspended 3/26/2014 – C400347-01, 02, 03, 04, 05, 06, 07 and 08 • Residue, Settleable 3/25/14 – C403542-01, 02, 03 and 04 • Specific Conductivity 3/18/14 – C401439-03 • Total Kjeldahl Nitrogen – 4E30003 Page 15 #591 – Environmental Conservation Laboratories, Inc. No transcription errors were detected. The facility appears to be doing a good job of accurately transcribing data. V. CONCLUSIONS: We are concerned with the finding that was cited previously and not corrected. Correcting the above-cited findings and implementing the recommendations will help this lab to produce quality data and meet certification requirements. The inspector would like to thank the staff for its assistance during the inspection and data review process. Please respond to all findings. Report prepared by: Nick Jones Date: October 9, 2014 Report reviewed by: Todd Crawford Date: October 10, 2014 Page 16 #591 – Environmental Conservation Laboratories, Inc. Matrix Spiking (NC WW/GW LC Policy 05/11/2012) Unless the referenced method states a greater frequency, spike 5% of samples on a monthly basis. Laboratories analyzing less than 20 samples per month must analyze at least one matrix spike (MS) each month samples are analyzed. If MS results are out of control, the results must be qualified or the laboratory must take corrective action to rectify the effect, use another method, or employ the method of standard additions. When the method of choice specifies MS performance acceptance criteria for accuracy, and the laboratory chooses to develop statistically valid, laboratory-specific limits, the laboratory-generated limits cannot be less stringent than the criteria stated in the approved method. When spiking with multi-component standards, if the method does not specify the spiking components, the Laboratory Control Spike (LCS) and MS must contain all analytes that are reported. If the unspiked sample result is in the top 40% of the calibration range, the sample should be diluted and the MS prepared using the diluted sample. The recovery of the MS samples must be bracketed by the calibration range. The volume of spike solution used in MS preparation must in all cases be ≤ 10% of the total MS volume. It is preferable that the spike solution constitutes ≤ 1% of the total MS volume so that the MS can be considered a whole volume sample with no adjustment (i.e., volume correction) by calculation necessary. If the spike solution volume constitutes >1% of the total sample volume, the sample concentration or spike concentration must be adjusted by calculation. Parameters Excluded from MS Requirements Acidity Alkalinity BOD/CBOD Aquatic Humic Substances Chlorophyll All Bacteriological Parameters Color – ADMI Color - PtCo Conductivity Dissolved Oxygen Ignitability All Residues Paint Filter Test Turbidity pH Temperature Salinity Sulfite Total Residual Chlorine Vector Attraction Reduction (All Options) (Field Laboratories and Field Setting analyses are exempt.) Page 17 #591 – Environmental Conservation Laboratories, Inc. Total Solids and Total Dissolved Solids Reporting Limit (NC WW/GW LC Policy 9/29/2014) Choose sample volume to yield between 2.5 and 200 mg dried residue. To obtain the required residue yield, successive aliquots of samples may be added to the same dish after evaporation or adjust reporting level based upon the weight gain and sample volume used. For example, if 100 mL sample is analyzed, and less than 2.5 mg of dried residue is obtained, the value reported would be <25 mg/L. The minimum reporting value is established at 2.5 mg/L based upon a sample volume used of 1000 mL. Total Suspended Solids Reporting Limit (NC WW/GW LC Policy 9/25/2014) The minimum reporting value is established at 2.5 mg/L when 1000 mL of sample is analyzed. The minimum weight gain allowed by any approved method is 2.5 mg. In instances where the weight gain is less than the required 2.5 mg, the value must be reported as less than the appropriate value based upon the volume used. For example, if 500 mL of sample is analyzed and < 2.5 mg of dried residue is obtained, the value reported would be < 5 mg/L. Page 18 #591 – Environmental Conservation Laboratories, Inc. Page 19 #591 – Environmental Conservation Laboratories, Inc.