HomeMy WebLinkAboutNC0020117_Lundy's Lab Inspection_20011004Michael F. Easley, Governor
William G. Ross Jr., Secretary
North Carolina Department of Environment and Natural Resources
Gregory J. Thorpe, Ph.D.
Acting Director
Division of Water Quality
October 4, 2001
116
Ms. Karen Autry
The Lundy Packing Co.
P.O. Box 49
424 Railroad Street
Clinton, NC 28328-0049
SUBJECT: Laboratory Certification Maintenance Inspection
Dear Ms. Autry:
�Ci 8 2001
Enclosed is a report for the inspection performed on September 20, 2001 by Mr.
Frederick L. Bone. Within thirty days, please supply this office with a written item for item
description of how these deficiencies were corrected. Unless specifically requested, a
response is not required for comments or recommendations. If the deficiencies cited in
the enclosed report are not corrected, enforcement actions will be recommended. For
certification maintenance, your laboratory must continue to carry out the requirements set
forth in 15A NCAC for 2H .0800.
Copies of the checklists completed during the inspection may be requested from
this office. Thank you for your cooperation during the inspection. Please contact us at
919-733-3908, if you have questions or need additional information.
Sincerely,
James W. Meyer
Laboratory Section
Enclosure
cc: Frederick L: Bone
Fayetteville Regional Office
tN��DENR
Laboratory Section N. C. Division of Water Quality 1623 Mail Service Center Raleigh, NC 27699-1623 (919) 733-3908
FAX: 919-733-6241 Internet: www.esb.enr.state.nc.us/lab
On -Site Inspection Report
LABORATORY NAME: Lundy Packing Co.
ADDRESS:
CERTIFICATE NO:
DATE OF INSPECTION:
TYPE OF INSPECTION:
EVALUATOR:
P.O. Box 49
424 Railroad Street
Clinton, NC 28328
116
September 20, 2001
Maintenance
Frederick L. Bone
LOCAL PERSON(S) CONTACTED: Karen Autry, Susan Melchor
1. 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 laboratory is spacious. and .well equipped. All facilities and equipment are well maintained.
Records are well kept and most data looked good. Some further quality control procedures need to be
implemented.
III. DEFICIENCIES, RECOMMENDATIONS, REQUIREMENTS, AND COMMENTS:
General:
1. DEFICIENCY: The laboratory is not performing sufficient quality control for it's duplicate sample
analyses. The laboratory must calculate either the relative percent difference, or the absolute
difference for each duplicate pair analyzed. This value is then used to establish control charts or
other appropriate acceptance criteria. This type of data is necessary to demonstrate that the data is
within acceptable control limits. The %RPD must be listed on the inorganic benchsheets so that the
analyst will be able to immediately confirm whether or not the data falls within acceptable limits.
REQUIRE MENT: Any time quality control results indicate an analytical .problem, the problem must be
resolved, and any samples involved, must be rerun if the holding time has not expired. Ref: 15A
NCAC 2H .0805 (a) (7) (f). .
2. DEFICIENCY: The laboratory is not verifying the automatic temperature compensation of the pH
meter on an annual basis.
Page 2
REQUIREMENT: All thermometers must meet National Institute of Standards and Technology
(NIST) specifications for accuracy or be checked against a NIST traceable thermometer and proper
corrections made. Ref: 15A NCAC 2H .0805 (a) (7) (o).
3. DEFICIENCY: The laboratory is using a temperature range of 3-5°C for sample refrigerators.
COMMENT: The laboratory may use a temperature range of 1-4°C, this will allow for the use of the
current thermometer in the sample refrigerator. This sample thermometer is graduated in 0.5 °C
increments.
REQUIREMENT: The acceptable temperature range of samples during storage and for stored sample
extracts, is 1.0-,4.4°C. Ref: Federal Register, July 1,:1995; 40 CFR 136; Table II. Required Containers,
Preservation Techniques, and Holding Times. EPA letters of January and February 1995.
A. COMMENT: The laboratory keeps a log for the preparation of standards and reagents. The logs
that are maintained donot contain all of the necessary information and need to be further expanded.
REQUIREMENT: The laboratory must have a written record of all standardsand reagents on file for
a period of at least five years (in accordance with temporary Certification Rule effective 10/01/2001.
A standard and reagent logbook will help the laboratory to meet this requirement. A standards
logbook will also enable the laboratory to document exactly when, by whom, and exactly how each
reagent is prepared.
B. COMMENT: The thermometer in the drying oven is currently reading the internal air temperature
and not the sample matrix temperature.
RECOMMENDATION: The thermometer in the drying oven should be placed in a beaker of sand or
other solid matrix. This ensures that the proper matrix temperature is measured as well as providing
a more stable temperature environment for the thermometer readings.
C. COMMENT: The laboratory does not list the acceptance ranges of quality control samples on the
benchsheets.
RECOMMENDATION: It is strongly recommended that the laboratory,list the acceptance ranges for
each quality control sample on the benchsheet. This will enable the analyst to compare the analytical
result to the acceptable range in a timely fashion. If the sample is out of the acceptable range, it can
then be reanalyzed immediately and within all holding times.
D. COMMENT: The laboratory is notrunning a second. source QC standard for all of its parameters.
REQUIREMENT: Analyze one known standard in addition to calibration standards each day samples
are analyzed to document accuracy. This LCS (laboratory control standard) must be from a second
source. For held curves for colorimetric methods, it must be analyzed after the initial CCV (continuing
calibration verification standard) is analyzed. It is recommended that this laboratory control standard,
like the CCV, have a mid -range concentration and not vary by more than ± 10%. If it does, the
analysis is out of control. The analysis must be terminated and the problem corrected. Ref: 15A
NCAC 2H .0805 (a) (7) (B), (F), and Standard Methods, 18th Edition - Method 1020 B.3.
Page 3
E. COMMENT: The laboratory is using a benchsheet that contains information for several parameters
on a single sheet of paper. Using this . method of data recording does not allow adequate space to
record all of the necessary quality control information for each parameter.
RECOMMENDATION: It is strongly recommended that the laboratory use one benchsheet for each
parameter analyzed. This will allow for all of the necessary quality control information for each
parameter to be recorded in a clear and concise manner.'
F. COMMENT: Some of the daily logs and benchsheets used by the laboratory do not contain' all of
the necessary labeling information. No units of measure are associated with some of the data values
listed in the logbooks and on the laboratory benchsheets.
REQUIREMENT: The laboratory must review all benchsheets and logbooks to ensure that every
entry is marked with the appropriate units of measure. Every number recorded on a benchsheet or
logbook must have an appropriate unit assigned to it.
G. COMMENT: Duplicates are not clearly labeled on the laboratory benchsheets..
RECOMMENDATION: For duplicate samples, the sample name should be followed by the term
"Dup" or "Duplicate" to indicate sample duplication. This will clearly delineate duplicate samples from
regular samples.
Fecal Coliform (MPN):
H. COMMENT: The laboratory does not analyze any samples for this parameter. The equipment
needed to perform this analysis is currently stored in boxes in the laboratory.
RECOMMENDATION: The laboratory may seriously consider . removing this parameter from it's
certified parameter list. NO analysis in the past year and the cost of maintaining chemicals and
performance evaluation samples for this parameter make MPN coliform analysis impractical for this
facility.
Total Suspended Solids:
I. COMMENT: The laboratory performs an annual drying time verification study. When the study is
conducted, the laboratory does not record the time that the samples were placed into and were taken
out of the oven. The laboratory does list that the samples were in the oven for 1,2,3 hours etc. , but
no times are associated with these hours.
REQUIREMENT: The laboratory must list the times that samples were placed into and were taken
out of the -drying oven for the annual drying time verification: study. This will allow the laboratory to
verify the actual time that samples were in the drying oven.
J. COMMENT: The laboratory does not record the time that samples are placed into the oven or
removed from the oven on the daily worksheet.
REQUIREMENT: The time in and out of the drying oven must.be documented to verify drying time is
adequate. .
Page 4
K. COMMENT: The laboratory is not analyzing a weight in the Tess than one gram range quarterly.
REQUIREMENT: An analytical balance capable of weighing 0.1 mg is required for certification. Ref:
15A NCAC 2H .0805 (a) (6) (d). The balance must be calibrated with class "S", "1". or "2" weights to
bracket the range of the instrument.
L. COMMENT: The laboratory is not analyzing water blanks for the Total Suspended Solids analysis.
The laboratory must filter a volume of DI water (equal to the maximum. sample volume used) as a
method blank each analysis day.
REQUIREMENT: Blanks must be analyzed in order to determine bias in each sample batch: Ref:
Standard Methods 18th Edition - Method 1020B pg. 1-5.
M. COMMENT: The amount of sample filtered for each duplicate analysis is not consistent. The
laboratory varies the amount of sample filtered from one duplicatesample to the next.
REQUIREMENT: the laboratory must filter the exact same amount of sample for each duplicate
analysis.
COD:
4. DEFICIENCY: The laboratory is not analyzing and recording a standard at the mid -range of the
calibration curve daily. The laboratory is analyzing a 4 point analytical curve each analysis day, but
does. not reanalyze a mid -point check standard daily.
COMMENT: As was discussed at the time of the audit the mid -range is to be defined, for all samples,
as one half the concentration of the high standard.
Note: The mid -range check standard must be prepared from the same stock standards as the
analytical curve. A second source laboratory control standard (LCS) must be analyzed in addition to
the mid -range check standard daily. A second source LCS sample does not constitute daily mid-
range verification.
REQUIREMENT: The laboratory must _analyze a 500 mg/L standard in addition to the 4 point
calibration curve daily. This standard must recover within 10% of the true value. Verify the standard
curve daily by analyzing one or more standards. within the linear range, as specified in the individual
method. The curve must be updated as set forth in the standard procedures, each time the slope
changes by more than 10 percent at midrange. Ref: Standard Methods 18th Edition 1020 B. Quality
Control section 5 p. 1-5, and Ref: 15A NCAC 2H .0805 (a) (7) (i).
N. COMMENT: The laboratory does not record the time on and time off of the samples in the COD
reactor.
RECOMMENDATION: It is strongly recommended that the laboratory record the time that the
samples were placed into the reactor and removed from the reactor in order to verify that the
samples were digested for the appropriate amount of time.
Page 5
O. COMMENT: The blank for the COD analysis is not clearlylabeled on the daily benchsheets.
REQUIREMENT: The laboratory. must clearly label and record the blank on each COD benchsheet.
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. Ref: 15A NCAC 2H .0800 (a) (7) (h).
P. COMMENT: The laboratory is currently analyzing a 4 point analytical curve daily.
RECOMMENDATION: The needs of the laboratory may be better served by analyzing a 5 point
analytical curve annually, rather than a 4 point curve daily.
Q. COMMENT: The laboratory does not demonstrate linearity of the analytical curves: The laboratory
is not calculating correlation coefficients for the standard curves.
REQUIREMENT: The laboratory must calculate a correlation coefficient for each analytical .curve in
order to demonstrate linearity. Analytical Quality Control Program. 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. The quality control -document shall be available for inspection by the
State Laboratory. Ref: 15A NCAC 2H .0805 (a) (7).
R. COMMENT: The laboratory . does not analyze low-level HACH tubes or maintain a low-level
analytical curve for COD analysis. The laboratory only has'high level tubes on site.
RECOMMENDATION: The laboratory must obtain low level COD vials and perform a low level
analytical curve in order to accurately report samples less than 150mg/L.
Oil and Grease:
5. DEFICIENCY: The laboratory is analyzing an extracted water blank not a Freon blank.
Note: Since no water is introduced into .the extraction, the blank used for this method must be a
solvent blank. The Freon blank value may be used for the entire lot of Freon. A new Freon blank
must be analyzed with each lot of Freon. .
REQUIREMENT: The value of the Freon blank must be subtracted from sample value in order to
obtain an accurate Oil and Grease result. Ref: Standard Methods 18th Edition 5520B p. 5-26.
6. DEFICIENCY: The laboratory is not properly measuring the amount of sample analyzed. .
REQUIREMENT: When a sample is brought into the laboratory, mark sample level on bottle for later
determination of sample, volume. To determine initial sample volume, fill sample bottle to mark with
water and then pour water into a 1-L graduated cylinder. Ref: Standard Methods, 18th Edition 5520B.
(4) p.5-26.
Page 6
BOD:
S. COMMENT: Some BOD blank values were not in the method accepted range of < 0.2 mg/L.
Note: The laboratory has extraordinarily high BOD samples. This leads to occasional contamination
of glassware. The laboratory is taking great care to prevent this problem. The laboratory may
consider a stronger acid for acid washing the glassware daily. A 20% solution of nitric acid may be
used daily to wash all BOD glassware.
REQUIREMENT: Blanks must be analyzed and calculated each analysis day. The DO uptake in 5d
at 20 °C should not be more than 0.2 mg/L and preferably not more than 0.1 mg/L. Standard
Methods, 18th Edition 5210B (4) (b) p.5-3.
7. DEFICIENCY: The laboratory GGA standards are frequently outside of the accepted range of 198
± 30.5 mg/L.
Note: The laboratory does not have to seed any samples. The only sample that is seeded is the
GGA. Currently the laboratory is only adding 1 milliliter of seed to the GGA sample. The laboratory
does not analyze any seed controls and thus does not have accurate information as to how much
seed is required in the GGA standard. The laboratory must calculate seed controls as described in
the method. The seed controls must provide a seed correction factor between 0.6 — 1.0 mg/L. From
this information, the laboratory will be able to determine the proper amount of seed to add to the
GGA sample thus stabilizing the results of the standard and achieving consistent, acceptable results.
REQUIREMENT: Use a mixture of 150-mg glucose/L and 150 mg glutamic acid/L as a standard
check. Determine the 5-d 20 °C BOD of a 2% dilution of the glucose glutamic acid standard check
solution. The average 5- d BOD would be 198 mg/L with a standard deviation of 30.5 mg/L. Ref:
Standard Methods, 18 Edition - Method 5210 pg. 5-3 to.5-5.
T. COMMENT: The laboratory is not currently performing an Oxidation and Reduction test for all
seeded samples. The laboratory must perform a titrametric analysis to determine the chlorine content
and neutralization for that chlorine for all BOD samples.
Note: This determination must be performed annually in order to demonstrate that no neutralization is
necessary. This site contains no Chlorine.
REQUIREMENT: The laboratory must perform Oxidation and Reduction tests for all seeded samples.
This is required by the method, in order to determine the amount of sodium sulfite or Potassium Bi-
iodate that is needed to neutralize the samples. The laboratory must perform the titrametric test for
the removal of residual chlorine, as described in Standard Methods, 18th Edition p 5-4.
U. COMMENT: The laboratory does not qualify data that does not meet established quality control
criteria.
Qualifying Versus Rejecting BOD Data
The- lab`is- not--_qualifyi_n_g_ the data _when__qua lity„dontrol _req.q.uirements .aret -met. _ L,Th.e=following
frformatron_rs-lifeMded CLenable-compliance: `�
Page 7
It is the desire. of the State of North Carolina that all data generated for any permitted location under
NPDES requirements is to be reported. " Every person subject to [15A NCAC 2B .0506] shall file
certified monitoring reports setting forth the results of tests and measurements conducted pursuant to
NPDES permitmonitoring requirements." Reference: 15A NCAC 2B .0506 (a) (1). Additionally, " the
results of all tests of the characteristics of the effluent, including but not limited to •NPDES Permit
Monitoring Requirements, shall be reported on monthly report forms." Reference: 15A NCAC 2B
.0506 (b) (3) (J).
The NPDES Permit itself states in Part II, Section D, Monitoring and Records, Number 7 - Recording
Results, " for each measurement or sample taken pursuant to therequirements of this permit, the.
permittee shall record the following information...the results of such analyses."
This means all data are reported and none are rejected. If all quality control requirements are not
met, it is required that the data be flagged and the qualification appear on the back of the Discharge
Monitoring Report (DMR). Any rejection of data from the storets will be issued by the agency that
receives the data:
The Quality Control requirements, of the method are outlined below:
1. The DO depletion of the dilution water blank must not be more than 0.2 mg/I.
2. The seed controls must deplete at least 2.0 mg/I. DO and have at least 1.0 mg/I DO remaining.
3. The samples must also deplete at least 2.0 mg/I DO and have at (east, 1.0 mg/I DO. remaining..
4. No evidence of toxicity should be present. This can only be evident when at least three dilutions
are analyzed. This is characterized by an increasing BOD value as the sample concentration
decreases.
5. The glucose glutamic acid standard must be in the acceptable range of 198 mg/I +/- 30.5 mg/I.
6. The seed correction, calculated from the seed controls, must be between 0.6 and 1.0 mg/I.
Anytime any of the above quality control requirements are not met, the data must be flagged. The
qualifying statement should. indicate that all QC requirements were not met. But the data must always
be reported.
V. COMMENT: The data is not presented in a clear and concise manner: Many items are not clearly
labeled and some analytical information is omitted.
RECOMMENDATION: The laboratory must review the BOD benchsheet and clearly label all
analytical information. List items such as calculations and acceptance criteria for the GGA standard
on the laboratory benchsheet. Be sure that no erroneous information is listed and that each number
has a unit of measure associated with it.
Ammonia=
8. DEFICIENCY: The laboratory is not distilling any samples, before analysis and has no comparative
data on file.
REQUIREMENT: To analyze samples without distillation, commercial laboratories shall accumulate
comparative data by analyzing at least six samples distilled and undistilled, but at least two samples
from all waste types. Analyze one sample distilled and undistilled yearly from all waste types.
t.
Page 8
Additional samples must be analyzed comparatively .if the above sample results do not indicate
approximately thesame values for distilled and undistilled samples.. Ref: Federal Register, January
31, 1994; 40 CFR 136; Footnote 6.
9. DEFICIENCY: The laboratory is not analyzing a blank daily.
REQUIREMENT: Analyze reagent blanks whenever new reagents are used and as often as required
in specific methods. Analyze a minimum of 5% of the sample loadas reagent .blanks; this monitors
purity of reagents and the overall procedural blank. Analyze a reagent blank after any sample with a
concentration greater than that of the highest standard or that might result in carryover from one
sample to the next. Ref: Standard Methods 18th Edition 1020B Quality Control (4) p 1-5.
W. COMMENT: The laboratory does not list the slope acceptance ranges of the electrode on the
analytical worksheet.
RECOMMENDATION: It is strongly recommended that the laboratory list the acceptance ranges for
each quality control measure on the benchsheet. This will enable the analyst to compare the
analytical result to the acceptable range in a timely fashion. If the sample is out of the acceptable
range, it can then be reanalyzed immediately and within all holding times.
X. COMMENT: The standard that the laboratory is analyzing and recording is not at the required mid-
range concentration of the calibration curve. As was discussed at the time of the audit the mid -range
is to be defined, for all North Carolina samples, as on half the concentration of the high standard.
Note: The laboratory must analyze a mid -point standard at 250 mg/L rather than the current
200mg/L.
REQUIREMENT: Verify the standard curve daily by analyzing one or more standards within the linear
range, as specified in the individual method. The curve must be updated as set forth in the standard
procedures, each time the' slope changes by more than 10 percent at midrange. Ref: Standard
Methods 18th Edition 1020 B. Quality Control section 5 p. 1-5, and Ref: 15A NCAC 2H .0805 (a) (7)
(I).
IV. CONCLUSIONS:
Correcting the above deficiencies and comments should help the laboratory to produce quality data
and meet certification requirements.
Please respond to all numbered Deficiencies and lettered Comments
cited insthis report.
Report prepared by: Frederick L. Bone 'Date: September 24, 2001