HomeMy WebLinkAbout#314 2006 On-Site Inspection Report
LABORATORY NAME: STL Pensacola
ADDRESS: 3355 McLamore Drive
Pensacola FL 32514
CERTIFICATE NO: 314
DATE OF INSPECTION: February 8-9, 2006
TYPE OF INSPECTION: Maintenance
EVALUATOR: Ray Boling and Tony Hatcher
LOCAL PERSON(S) CONTACTED: Lance Larson, Darlene Nelson, John Meade, VanDa Chea, Mandi Edwards,
Galina Khramova, Mary Goldman, Stephanie Bubien, Marina Ramos, Sharon Taber, Jim Barkhalter, Becky
Tremmel, Brandi Mellinger, John Reed, John Harris, Gary St. Pere, Karen Nall, Shelley Kealley, Kim Ayers, Steve
Wilhite, George Hayman, Walter Drew, David Bowery, Rita Wingo, Jane Schumann, Larry Dilmore, Isabel
Enfinger, Charlie Potts, Davette Havard, and Jeremy Bosso.
I. INTRODUCTION:
This laboratory was inspected to verify its compliance with the requirements of 15A NCAC 2H .0800 for the
analysis of environmental samples.
II. GENERAL COMMENTS:
The lab was spacious and well equipped. The facilities were well maintained. Records were well kept and
most data looked good. Some further quality control procedures need to be implemented
III. DEFICIENCIES, REQUIREMENTS, COMMENTS AND RECOMMENDATIONS:
REFRIGERATORS and WALK-IN REFRIGERATION
(A) COMMENT: During the inspection the auditor noticed some temperature excursions of refrigeration
units out of the required range.
REQUIREMENT: To assure NPDES compliance, sample storage temperature should not exceed 4.4°C.
The lower temperature limit is dictated by the requirement that NPDES samples must not be frozen. As a
guideline, the temperature requirements for microbiological samples and media storage in the 18th Edition
of Standard Methods specify 1°C to 4.4°C. This range meets the criteria for NPDES sample storage and
would be acceptable for NPDES compliance monitoring. This must be documented in a logbook or on a
worksheet. Ref: EPA Letters of January and February 1995 and August 1999; and the Federal Register;
July 1, 2005, and 15A NCAC 2H .0805 (a) (7) (J).
Examples:
Refrigerator/Walk-in Inspection Temperature Month/days out of Temperature Range 2006
Extractions 0.23 5°C Jan: 12; Feb: 3
Extractions 0.22 4.°C Jan: 14; Feb: 1
SC001 5°C Jan: 24; Feb: 7
SC003 5°C Jan: 23; Feb: 7
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STL Pensacola Laboratory
February 8-9, 2006
Wet Chemistry
ANALYTICAL MASSES
RECOMMENDATION: Clean the masses with a gentle flow of air to remove the dust.
COMMENT: The inspector discovered Class P masses for the following weight: 200 grams. For NC testing
you must use a better class mass.
REQUIREMENT: A class S or 1 or 2 weight must be weighed each day before balance is used and the
weighing documented in a log with the date and signature of the analyst. Once each quarter a series of at
least three class S or 1 or 2 weights, covering the range of normal use for the balance, must be weighed
and documented in the log. Ref: NCAC 15A 2H (a) (7) (K).
NCLC Policy: Certified analytical weights, Class S, 1 or 2, must be recalibrated and recertified a
minimum of every 5 years.
BOD, 5-DAY
(1) DEFICIENCY: The initial DOs of the dilution water and samples were not less than 9 mg/L.
REQUIREMENT: The initial DO of the dilution water and samples must fall in the range of 7 to 9 mg/L. Ref:
Standard Methods 18th and 19th Editions, Method 5210 B. 6. b.
REQUIREMENT: The analyst must “Bring samples to 20 ± 1°C before making dilutions.” Ref: Standard
Methods 20th Edition, Method 5210 B. page 5-5, 5.
COMMENT: The inspector found initial DOs of 9.20 and 9.13 in the 11/23/2005 data. The bench sheet
listed the following: ‘Initial DO cannot be >9.3 mg/L at 20°C.’
INORGANIC PHENOLS, TOTAL PHOSPHORUS, ORTHOPHOSPORUS, NITRATE PLUS NITRITE,
TKN, AMMONIA NITROGEN,ION CHROMATOGRAPHY, EPA Method 300, COLOR (Pt/Co Method)
(B) COMMENT: The analyst did not test a mid-range, mid-concentration, standard each analysis day for
chloride and sulfate. Cited Previously
REQUIREMENT: The mid-range standard must be analyzed each analysis day and must be at or near the
mid-range of the curve. The percent recovery must be documented on the worksheets. A second-source
standard must be analyzed with each batch of samples. Ref: NCAC 15A 2H .0805 (a) (7) (I) and Standard
Methods 18th Edition; Method 1020 B. and C., 1030 C., 3020, Quality Control, page 3-3
SPECIFIC CONDUCTIVITY
(C) COMMENT: You listed your lower reporting limit (LRL) as 1 µmhos/cm on the bench sheet. On the NC
application you listed 14.9 µmhos/cm.
For chloride by the automated method, your standard curve started at 2 mg/L. We do not know what your
LRL will be for NC samples.
REQUIREMENT: You must reply what your lower reporting limit will be for NC samples.
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STL Pensacola Laboratory
February 8-9, 2006
COLOR, Platinum/Cobalt Method, EPA 110.1
(D) COMMENT: The curve printout listed color sample values in mg/L instead of Color Units.
REQUIREMENT: All laboratories must use printed laboratory bench worksheets. These documents must
include a space to enter the value from the measurement system and each item must be recorded each
time samples are analyzed. This must be documented. Ref: 15A NCAC 2H .0800 - section .0805 7 H.
REQUIREMENT: The laboratory must document all relevant information. If the information is not recorded,
the laboratory has no means to prove that the procedure was actually performed.
COMMENT: Data reviewed: 3/27/2004 and 10/12/2005.
MBAS, EPA Method 425.1
(2) DEFICIENCY: The analyst did not test a standard at the lower reporting limit of 0.1 mg/L. Cited
Previously
REQUIREMENT: For analytical procedures requiring analysis of a series of standards, the concentrations
of these standards must bracket the concentration of the samples analyzed. One of the standards must
have a concentration equal to the Laboratory's lower reporting concentration for the parameter involved.
Curves prepared annually must consist of at least 5 standard concentrations and a blank. Curves prepared
daily must consist of at least three standard concentrations and a blank. Ref: 15A NCAC 2H .0805 (a) (7)
(I) and Standard Methods, 18th Edition, Method 1020 B. 5.
OIL & GREASE, EPA Method 9071B
(3) DEFICIENCY: The analyst used magnesium sulfate with the soil and sediment samples. Cited
Previously
REQUIREMENT: Sodium Sulfate must be mixed with the soil or sediment samples before extraction. Ref:
EPA Method 9071B; 11.2.2.2
SULFITE, EPA Method 377.1 or SM 4500 SO3=
COMMENT: The inspector reviewed data for sulfite that was not ‘flagged’ as out of the holding time as
listed in the Federal Register. Lab staff indicated that the new lab software will automatically ‘flag’ data out
of the holding time.
(4) DEFICIENCY: During review of data from 12/25/2005 the inspector discovered a LCS (20 mg/L)
recovery (82.5%) out of the labs quality control limits of 85-115%.
REQUIREMENT: Analyze a blank and check standard containing the analyte of interest at a frequency of
each batch. Document the percent recovery on the worksheet. The recovery must be within ± 10%. Ref:
Federal Register, 40 CFR-136 Appendix C 7.6.1 and 12.1.1c, Standard Methods 18th Edition, Method
1020 B. and C., 1030 C., 3020, Quality Control, page 3-3
SULFATE, EPA Method 375.4
(5) DEFICIENCY: The analyst did not construct the calibration curve with a 5-mg/L interval among all
calibration standards.
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STL Pensacola Laboratory
February 8-9, 2006
REQUIREMENT: 6.3.2 ‘Space standards at 5 mg/L increments in the 0-40 mg/L sulfate range.’ Ref: EPA
Manual Revision March 1983, Method 375.4, 6.3.2
COMMENT: The curve was the following: 5, 10, 15, 20, 25, 30 and 40 mg/L.
SETTLEABLE RESIDUE, Imhoff Cone Method
(6) DEFICIENCY: The analyst did not document that the sample settled for 45 minutes and then an
additional 15 minutes before the analysis was complete.
REQUIREMENT: “Fill an Imhoff cone to the 1-L mark with a well-mixed sample. Settle for 45 minutes,
gently agitate sample near the sides of the cone with a rod or by spinning, settle 15 minutes longer, and
record volume...” Ref: Standard Methods 18th Edition; Method 2540 F. 3. Procedure
TCLP, Method 1311 and 1312
(E) COMMENT: The analyst did not rotate samples again if the minimum pressure was not met at the end
of the first rotation.
REQUIREMENT: The analyst must bring the ZHE to 50 psi in order to begin the leaching of the sample(s).
The analyst must maintain this pressure until the end of the rotation. Ref: SW846 Method 1311, Section
7.3.8
COMMENT: The analyst and supervisor agreed to rotate samples again if the minimum pressure required
by the method was not met at the end of the first tumble for NC samples.
RECOMMENDATION: Replace all pH standard buffer solutions at the end of each analysis day.
Metals Laboratory
EPA Method 1631E, Low-Level Mercury Method
(F) COMMENT: The analyst did not provide the information of the collection time of the 1631 samples on
the worksheet in order to meet the 48-hour holding time for unpreserved samples.
REQUIREMENT: 8.5.1 ‘Samples to be analyzed for total or dissolved Hg only may be shipped to the
laboratory unpreserved and un-refrigerated if they are collected in fluoropolymer or glass bottles and
capped tightly. Samples must be either preserved or analyzed within 48 hours of collection. If a sample is
oxidized in the sample bottle, the time to preservation can be extended to 28 days.’ Ref. EPA Method
1631, Revision E, page 14, 8.5.1
NORTH CAROLINA DENR/DWQ
WASTEWATER/GROUNDWATER
LABORATORY CERTIFICATION
MEMORANDUM
DATE: August 18, 2004
TO: All labs certified for EPA Method 1631
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STL Pensacola Laboratory
February 8-9, 2006
FROM: James W. Meyer
SUBJECT: Preservation
There appears to be confusion about how the samples are to be preserved and when to preserve them.
The letter from Gary Bennett of EPA Region IV seems to give the impression that if the BrCl is added to
the original collection bottle, that samples do not need to be preserved further. In researching this issue it
becomes clear that Mr. Bennett’s letter is being misinterpreted.
The Method clearly states in Section 8.5.1 that “Samples must be either preserved or analyzed within 48
hours of collection. If a sample is oxidized in the sample bottle, the time to preservation can be extended to
28 days.”
Note 17 referred to in the letter states that “Samples collected for the determination of trace level mercury
using EPA Method 1631 must be collected in tightly-capped fluoropolymer or glass bottles and preserved
with BrCl or HCl solution within 48 hours of sample collection. Samples for dissolved trace level mercury
must be filtered in a clean area in the field or in the laboratory prior to preservation. Samples that have
been preserved for determination of total or dissolved trace level mercury must be analyzed within 90 days
of sample collection.”
The determination of this office is that the oxidation process with BrCl to delay preservation must begin at
the time of collection. Hence, the collection bottle must contain the BrCl at time of collection, the BrCl
added to the bottle immediately upon collection or the samples must be shipped immediately to the lab
and the BrCl added within 48 hours of collection. The lab then has 28 days in which to complete the
preservation. If this process is delayed for more than 48 hours, the samples must be discarded or qualified
as not having met preservation and/or holding times and this office must be notified in writing of the non-
compliance.
COMMENT: The analyst did not condition the sample trap with a series of replicates of the 0.5 ng/L
standard before data collection of samples began.
RECOMMENDATIONS: (a) Test multiple 0.5 ng/L standards to condition the sample trap before analysis
and data collection begins.
(b) Use more than one replicate for each standard and sample along with the initial calibration.
Mercury by Cold Vapor Method
(G) COMMENT: The analyst did not test a mid-range, mid-concentration, standard each analysis day.
REQUIREMENT: The mid-range standard must be analyzed each analysis day and must be at or near the
mid-range of the curve. The percent recovery must be documented on the worksheets. A second-source
standard must be analyzed with each batch of samples. Ref: NCAC 15A 2H .0805 (a) (7) (I) and Standard
Methods 18th Edition; Method 1020 B. and C., 1030 C., 3020, Quality Control, page 3-3
ALL METALS ANALYSES
COMMENT: Laboratory personnel cannot report NC samples to values below the lower reporting limit
(LRL) such as your MDL.
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STL Pensacola Laboratory
February 8-9, 2006
Organic Chemistry Laboratory
PURGEABLE ORGANIC CHEMISTRY, EPA Method 602
(7) DEFICIENCY: The analyst does not spike 10% of samples.
REQUIREMENT: "The laboratory must, on an ongoing basis, spike at least 10 % of the samples from each
sample site..." Ref: Federal Register; 40 CFR Part 136, App. A, Method 602; page 340; 8.1.4
RECOMMENDATION: Do not delete the lowest point in an initial calibration curve in order to meet the
requirements of linearity of the standard curve.
EPA Method 608, Organochlorine Pesticides
(8) DEFICIENCY: The analyst does not spike 10% of samples as MS/MSD pairs.
REQUIREMENT: "The laboratory must, on an ongoing basis, spike at least 10 % of the samples from each
sample site..." Ref: Federal Register; 40 CFR Part 136, App. A, Method 608; page 413; 8.3
STRONG RECOMMENDATION: If the RSD of any verification standard analyte is >15% and the analyte
was detected in the sample, the analyst should reanalyze or reextract the sample. If the analyst just flags
the sample result, this is not good chemistry.
RECOMMENDATION: The analyst should be using the method quality control limits, 70-130%, for the
LCS and the MS/MSD limits until sufficient lab data is generated to provide laboratory limits based on
matrix and at least 20 to 30 duplication/spiking results.
EPA Method 610 and 8310 by HPLC, Polynuclear Aromatic Hydrocarbons
(H) COMMENT: For aqueous samples the analyst did not test 5% of all samples as matrix spike and
matrix spike duplicate pairs. And, (6) DEFICIENCY: The analyst did not test a mid-range, mid-
concentration, verification standard each analysis day. The analyst did not test a second source
standard each analysis day.
REQUIREMENT: 8.4.1 “The reference sample concentrate must be made using stock standards prepared
independently from those used for calibration.” Ref: SW846; Method 8000B; page 8000 B - 37
REQUIREMENT: 8.5 “The laboratory must also have procedures for documenting the effect of the matrix
on method performance (precision, accuracy, and detection limit). At a minimum, this will include the
analysis of at least one matrix spike and one duplicate unspiked sample or one matrix spike/matrix spike
duplicate (MS/MSD) pair with each batch of up to 20 samples of the same matrix processed together (see
Chapter One).
If samples are expected to contain the target analytes of concern, then laboratories may use one matrix
spike and a duplicate analysis of an unspiked field sample as an alternative to the MS/MSD pair (see
Section 8.5.3).” Ref: SW 846; EPA Method 8000B; pages 8000B - 39-42.
REQUIREMENT: The mid-range standard must be analyzed each analysis day and must be at or near the
mid-range of the curve. The percent recovery must be documented on the worksheets. A second-source
standard must be analyzed with each batch of samples. Ref: NCAC 15A 2H .0805 (a) (7) (I) and Standard
Methods 18th Edition; Method 1020 B. and C., 1030 C., 3020, Quality Control, page 3-3
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STL Pensacola Laboratory
February 8-9, 2006
PURGEABLE ORGANIC CHEMISTRY, EPA Method 624/8260/6210D
RECOMMENDATION: For aqueous samples you can maintain a low-range and a hi-range calibration
curve for GC/MS.
IV. PAPER TRAIL INVESTIGATION: This consisted of reviewing data reported on the laboratory bench
sheets. Data reviewed for the clients Pope AFB for May of 2005 indicated some problems in proper data
reporting.
Client: Pope Air Force Base
Collected: May 18, 2005
Received: May 19, 2005
Tests requested: Oil and Grease, 1664; MBAS 425.1; EPA Method 610, PAH’s; EPA Method 239.2, Lead
by Furnace AA
Received at 7.7°C in STL receiving room.
(I) COMMENT: Client Problem: The client did not provide sufficient water ice for cooling the samples to
4°C during transport.
REQUIREMENT: Client Problem: The acceptable temperature range of samples during transportation is
0.1°C to 6°C. Ref: Federal Register, July 1, 2005; 40 CFR 136; Table II. Required Containers,
Preservation Techniques, and Holding Times. EPA letters of January and February 1995. (Given to lab at
time of inspection.)
REQUIREMENT: STL personnel must send a notification letter to the State of NC when a client
does not meet the federal register requirement for the transportation of samples at 4°C.
V. CONCLUSIONS:
We are concerned with the deficiencies that were cited previously and not corrected. Failure to correct the
deficiencies cited in this report will lead to enforcement action.
Ref: 15A NCAC 2H .0807 (a) (1) and (14)
Laboratory Decertification:
A laboratory may be decertified for any or all parameters for up to one year for any or all of the following
infractions:
(1) Failing to maintain the facilities, or records, or personnel, or equipment, or quality control
program as set forth in the application, and these Rules; or
(14) Failing to comply with any other terms, conditions, or requirements of this Section or of a
Laboratory certification.
Correcting the above cited deficiencies and comments and implementing the recommendations will
help this lab to produce quality data and meet certification requirements. Please respond to all
numbered deficiencies and lettered comments.
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STL Pensacola Laboratory
February 8-9, 2006
VI. OBSERVATIONS, STATEMENTS AND QUESTIONS:
COMMENT: The analyst must check the temperature compensation feature of each meter containing a
temperature compensation device annually,
REQUIREMENT: (New Policy) Automatic Temperature Compensator Check (ATC) for pH meter
and Conductivity meter: (Check every 12 months)
1. Take a buffer or standard solution and cool to below 10ºC and read the temperature. Analyze the
buffer or standard solution at that temperature. Document the temperature and the measured pH or
standard solution value obtained on the log sheet.
2. Raise the temperature of the buffer or standard solution to approximately 25ºC. Document the
temperature and the measured pH or standard solution value on the log sheet.
3. Raise the temperature of the buffer or standard solution to approximately 35ºC. Document the
temperature and the measured pH or standard solution value on the log sheet.
4. Repeat with additional temperature adjustments and pH or standard solution readings as necessary
to ensure the temperature usually measured for samples has been bracketed. As the temperature
increases or decreases the value of the buffer or standard solution should remain approximately the
same.
REQUIREMENT: (New Policy) Temperature Sensor Check (pH meter/ DO meter/Conductivity)
(Check every 12 months)
To check the temperature sensor read the temperature of the meter against a NIST thermometer and
record the two temperatures. It is recommended that the correction factor be no more than 1 degree.
The correction factor must be less than 3º C. In the documentation include the serial number of the
NIST thermometer or traceable thermometer that was used in the comparison. Also document any
correction that applies on both the instrument and on a separate sheet to be filed.
REQUIREMENT: The temperature sensor must be calibrated annually even if it is not being used
to report temperature.
Report prepared by: Ray Boling Date: June 23, 2006