HomeMy WebLinkAbout#330_2016_0218_NJ_FINALREPORTINSPECTION ROUTING
To be attached to all inspectionreports
Laboratory Cert. #:
330
Laboratory Name:
PCS Phosphate Company, Inc.
Inspection Type:
Industrial Maintenance
Inspector Name(s):
Nick Jones
Inspection Date:
February 18, 2016
Date Report Completed:
March 3, 2016
Date Forwarded to Reviewer:
March 3, 2016
Reviewed by:
Tonia Springer
Date Review Completed:
March 3, 2016
Cover Letter to use:
❑ Insp. Initial ❑ Insp. Reg.
❑ Insp. No Finding ❑ Insp. CP
® Corrected
Unit Supervisor/Chemist III:
Todd Crawford
Date Received:
March 9, 2016
Date Forwarded Admin:
March 21, 2016
Date Mailed:
March 21, 2016
i✓b'caPer Resources
EN` IRONMEN I AL QUALITY
March 21, 2016
330
Ms. Pamela Jestness
PCS Phosphate Company, Inc.
1530 NC Hwy 306 South
Aurora, NC 27806
PAT MCCRORY
DONALD R. VAN DER VAART
S. JAY ZIMMERMAN
SUBJECT: North Carolina Wastewater/Groundwater Laboratory Certification (NC WW/GW LC)
Maintenance Inspection
Dear Ms. Jestness:
Enclosed is a report for the inspection performed on February 18, 2016 by Mr. Nick Jones. Since the
Finding(s) cited during the inspection were all corrected prior to the completion of the enclosed report, a
response is not required. The staff is commended for taking the initiative in correcting the Findings in
such a timely manner. For Certification maintenance, your laboratory must continue to carry out the
requirements set forth in 15A NCAC 2H .0800.
Copies of the checklists completed during the inspection may be requested from this office. Thank you
for your cooperation during the inspection. If you wish to obtain an electronic copy of this report by
electronic mail, or if you have questions or need additional information, please contact me at (919) 733-
3908 ext. 251.
Sincerely,
Todd Crawford
Technical Assistance & Compliance Specialist
NC WW/GW Laboratory Certification Branch
Attachment
cc: Dana Satterwhite; Nick Jones;
WaRO; Master File #330
Water Sciences Section
NC Wastewater(Groundwater Laboratory Certification Branch
1623 Mail Service Center, Raleigh, North Carolina 27699-1623
Location: 4405 Reedy Creek Road; Raleigh, North Carolina 27607
Phone: 919-733-39081 PAX: 919-733-6241
Internet: http://deq.nc.gov/abouVdivisionstwater-resources/water-resources•data/wat rr•sciences•home-page/iaboratorv�cerfification-branch
LABORATORY NAME:
NPDES PERMIT #:
ADDRESS:
CERTIFICATE #:
DATE OF INSPECTION:
TYPE OF INSPECTION:
AUDITOR(S):
LOCAL PERSON(S) CONTACTED:
INTRODUCTION:
PCS Phosphate Company, Inc.
NC0003255
1530 NC Hwy 306 South
Aurora, NC 27806
330
February 15, 2016
Industrial Maintenance
Nick Jones
Pamela Jestness, Brad Lee,
Dale Davis, and John Braddy
This laboratory was inspected by a representative 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.
GENERAL COMMENTS:
The facility has all the equipment necessary to perform the analyses. Laboratory personnel
communicate well with sample collectors and coordinate sample analyses effectively to manage
workload and holding times.
Proficiency Testing (PT) samples for the 2016 proficiency testing calendar year have not yet been
analyzed. The laboratory is reminded that these results must be submitted to this office directly
from the vendor by September 30, 2016.
The laboratory is reminded that all changes made in response to the Findings,
Recommendations or Comments listed in this report must be incorporated in the Quality
Assurance (QA)/Standard Operating Procedures (SOP) document(s). The laboratory must
ensure the method is being performed as stated, references to methods are accurate, and the
QA and/or SOP document(s) is/are 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 policies will be implemented.
Contracted analyses are performed by Environmental Chemists, Inc. (Envirochem) (Certification
#94), Environmental Testing Solutions, Inc. (Certification #600) and Microbac Laboratories, Inc.
(Certification #11).
The laboratory requested the deletion of Settleable Residue Standard Methods, 2540 F-1997
(Aqueous) from their Certified Parameter List (CPL) since it is no longer required by their permit.
This deletion was made effective as of February 29, 2016.
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#330 PCS Phosphate Company, Inc.
Q • x fa silt'�
QUalitV COntr01
Comment: The laboratory needed to increase the documentation of purchased materials and
reagents. The NC WW/GW LC Policy states: All chemicals, reagents, standards and
consumables used by the laboratory must have the following information documented: Date
received, Date Opened (in use) Vendor Lot Number, and Expiration Date (where specified)
This information as well as the vendor and/or manufacturer, lot number, and expiration date
must be retained for primary standards chemicals reagents and materials used for a period of
five years. Consumable materials such as pH buffers, lots of pre -made standards and/or media,
solids and bacteria filters, etc. are included in this requirement. Acceptable corrective action
(i.e., the analyst began filling out a traceability log to document purchased materials and
reagents) was performed by the laboratory and approved by the auditor during the inspection. No
further response is necessary for this Finding.
Comment: The laboratory did not have a Standard Operating Procedure (SOP) for Proficiency
Testing (PT) samples. 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. Notification of
acceptable corrective action (i.e., submission of an SOP for PT samples) was received by email
on 3/1/2016 with an implementation date of 3/1/2016. No further response is necessary for
this Finding.
Chlorine, Total Residual — Standard Methods, 4500 Cl G-2000 (Aqueous)
Conductivity —Standard Methods, 2510 B-1997 (Aqueous)
Fluoride — Standard Methods, 4500 F- C-1997 (Aqueous)
pH — Standard Methods, 4500 H+B-2000 (Aqueous)
pH — SW846 9045 D (Non -Aqueous)
Phosphorus, Total — Standard Methods, 4500 P F-1999 (Aqueous)
Residue, Suspended —Standard Methods, 2540 D-1997 (Aqueous)
Temperature — Standard Methods, 2550 B-2000 (Aqueous)
Turbidi — EPA 180.1, Rev. 2.0, 1993 (Aqueous)
Comment: The laboratory benchsheets did not list the complete method references. This is
considered pertinent information. The North Carolina Administrative Code, 15A NCAC 2H .0805
(a) (7) (A) states: 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. Notification of
acceptable corrective action (i.e., submission of revised benchsheets including method
references) were received by email on 3/2/2016 with an implementation date of 3/3/2016. No
further response is necessary for this Finding.
Chlorine. Total Residual — Standard Methods, 4500 Cl G-2000 (Aqueous)
Comment: The benchsheet did not document the true value of the mid -range standard. This is
considered pertinent information. The North Carolina Administrative Code, 15A NCAC 2H .0805
(a) (7) (A) states: 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. Notification of
acceptable corrective action (i.e., submission of a revised benchsheet including the true value
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#330 PCS Phosphate Company, Inc.
of the mid -range standard) was received by email on 3/1/2016 with an implementation date of
3/1/2016. No further response is necessary for this Finding.
Fluoride —Standard Methods, 4500 F- C-1997 (Aqueous)
Comment: The lab is not submersing the electrode in the standards/samples before the stir bar is
activated. Standard Methods, 4500 F- C-1997. (4) (d) states: Immerse electrodes in each of the
fluoride standard solutions and measure developed potential while stirring on a magnetic stirrer.
Avoid stirring before immersing electrodes because entrapped air around the crystal can produce
erroneous readings or needle fluctuations. Notification of acceptable corrective action (i.e., a
statement that the lab does not activate the stir bar before the electrode is submersed in the
standards/samples) was received by email on 3/1/2016 with an implementation date of
2/29/2016. No further response is necessary for this Finding.
pH — Standard Methods, 4500 H+D-2000 (Aqueous)
Comment: The benchsheet did not document the value of the check buffer (true and obtained)
and units of measure. This is considered pertinent information. The North Carolina Administrative
Code, 15A NCAC 2H .0805 (a) (7) (A) states: 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. Notification of acceptable corrective action (i.e., submission of a revised benchsheet
including the true and obtained values of the check buffer and units of measure) was received
by email on 3/1/2016 with an implementation date of 3/1/2016. No further response is
necessary for this Finding.
pH — SW846 9045 D (Non -Aqueous)
Comment: The benchsheet did not document the true value of the check buffer. This is
considered pertinent information. The North Carolina Administrative Code, 15A NCAC 2H .0805
(a) (7) (A) states: 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. Notification of
acceptable corrective action (i.e., submission of a revised benchsheet including the true value
of the check buffer and units of measure) was received by email on 3/1/2016 with an
implementation date of 3/1/2016. No further response is necessary for this Finding.
Comment: The lab was not reporting the accompanying temperature of the sample during the pH
analysis. EPA SW-846 Test Methods for Evaluating Solid Waste, Physical/Chemical Methods;
3rd Edition, Method 9045 D, Section 7.2.5 states: Report the results as "soil pH measured in water
at _°C" where "_°C" is the temperature at which the test was conducted. Notification of
acceptable corrective action (i.e., submission of a revised benchsheet including the temperature
of the sample during analysis) was received by email on 3/3/2016 with an implementation date
of 2/29/2016. No further response is necessary for this Finding.
Phosphorus, Total — Standard Methods, 4500 P F-1999 (Aqueous)
Comment: The digital benchsheets/instrument printouts were not being initialed and dated. This
is considered pertinent information. The North Carolina Administrative Code, 15A NCAC 2H
.0805 (a) (7) (A) states: 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. Notification of
acceptable corrective action (i.e., a statement that the digital benchsheets/instrument printouts
will be initialed and dated) was received by email on 3/1/2016 with an implementation date of
3/1/2016. No further response is necessary for this Finding.
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#330 PCS Phosphate Company, Inc.
Comment: The lab was not preserving samples with sulfuric acid within 15 minutes of collection.
The Code of Federal Regulations, Title 40, Part 136; Federal Register Vol. 77, No. 97, May 18,
2012; Table 11, footnote 2 states: Preserve each grab sample within 15 minutes of collection.
For a composite sample collected with an automated sample (e.g., using a 24-hour composite
sample; see 40 CFR 122.21(g)(7)(i) or 40 CFR Part 403, Appendix E), refrigerate the sample at
<-6°C during collection unless specified otherwise in this Table II or in the method(s). For a
composite sample to be split into separate aliquots for preservation and/or analysis maintain
the sample at <_6°C unless specified otherwise in this Table 11 or in the method(s) until
collection, splitting and preservation is completed Add the preservative to the sample
container prior to sample collection when the preservative will not compromise the integrity of a
grab sample, a composite sample or aliquot split from a composite sample within 15 minutes of
collection. Notification of acceptable corrective action (i.e., a statement that the lab will preserve
samples with sulfuric within 15 minutes of collection) was received by email on 3/1/2016 with an
implementation date of 2/19/2016. No further response is necessary for this Finding.
Residue, Suspended - Standard Methods, 2540 D-1997 (Aqueous)
Comment: Filters were not weighed to constant weight prior to sample analysis, nor was a dry
filter blank analyzed with each set of samples. NC WW/GW LC Policy states: If pre -prepared
filters are not used, the method requires that filters must be weighed to a constant weight after
washing. Repeat cycle of drying, cooling, desiccating, and weighing until a constant weight is
obtained or until weight change is less than 4% of the previous weighing or 0.5 mg, whichever is
less. In lieu of this process it is acceptable to analyze a single daily dry filter blank to fulfill the
method requirement of drying all filters to a constant weight prior to analysis. Notification of
acceptable corrective action (i.e., a statement that the lab began analyzing a dry filter blank
daily) was received by email on 3/1/2016 with an implementation date of 2/19/2016. No further
response is necessary for this Finding.
pH - Standard Methods, 4500 H+B-2000 (Aqueous)
Comment: The units of measure for pH are not documented on the monitoring well benchsheet.
The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (H) states: 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. Notification of
acceptable corrective action (i.e., submission of revised benchsheets including units of measure
for pH) was received by email on 3/1/2016 with an implementation date of 3/1/2016. No further
response is necessary for this Finding.
Fluoride - Standard Methods, 4500 F- C-1997 (Aqueous)
Phosphorus, Total - Standard Methods, 4500 P F-1999 (Aqueous)
Comment: The lab was not analyzing a Laboratory Fortified Matrix Duplicate (LFMD) at the
required frequency. Standard Methods, 4020 B-2009, Rev. 2011, Table 4020: 1 and (2) (g) states:
When appropriate for the analyte (Table 4020:1), include at least one LFM/LFMD daily or with
each batch of 20 or fewer samples. Notification of acceptable corrective action (i.e., a statement
that the lab will analyze LFMDs at the required frequency) were received by email on 3/3/2016
with an implementation date of 3/3/2016. No further response is necessary for this Finding.
Comment: The laboratory was not analyzing a calibration blank and calibration verification
standard (mid -range) after every tenth sample and at the end of the sample group. Standard
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#330 PCS Phosphate Company, Inc.
Methods, 4020 B-2011. (2) (b) states: Verify calibration by periodically analyzing a calibration
standard and calibration blank during a run —typically, after each batch of ten samples and at the
end of the run. NC WW/GW LC Policy states: The calibration blank and calibration verification
standard (mid -range) must be analyzed initially (i.e., prior to sample analysis), after every tenth
sample and at the end of each sample group to check for carry over and calibration drift. If
either fall outside established quality control acceptance criteria, corrective action must be
taken (e.g., repeating sample determinations since the last acceptable calibration verification,
repeating the initial calibration, etc.). Notification of acceptable corrective action (i.e., a
statement that calibration verifications and blanks are being analyzed at the end of sample
groups and after every ten samples as well as benchsheets which accommodate the new
Quality Control [QC] requirements) were received by email on 3/1/2016 with an implementation
date of 2/29/2016. No further response is necessary for this Finding.
Chlorine, Total Residual — Standard Methods, 4500 Cl G-2000 (Aqueous)
Comment: The laboratory was not evaluating reagent blanks against the required acceptance
criterion. The NC WW/GW LC Approved Procedure for the Analysis of Total Residual Chlorine
document states: The concentration of reagent blanks must not exceed 50% of the reporting
limit (i.e., the lowest calibration or calibration verification standard concentration), unless
otherwise specified by the reference method, or corrective action must be taken. Notification of
acceptable corrective action (i.e., a statement that the lab has established a blank acceptance
criterion not to exceed 50% of the reporting limit, as well as submission of benchsheets which
document the new requirements) was received by email on 3/1/2016 with an implementation
date of 3/1/2016. All reagent blank data reviewed during the inspection met the required
acceptance criterion. No further response is necessary for this Finding.
Fluoride — Standard Methods, 4500 F- C-1997 (Aqueous)
Phosphorus, Total — Standard Methods, 4500 P F-1999 (Aqueous)
Comment: The laboratory was not evaluating blanks against the required acceptance criterion.
NC WW/GW LC Policy states: For analyses requiring a calibration curve, the concentration of
reagent, method and calibration blanks must not exceed 50% of the reporting limit or as
otherwise specified by the reference method. Notification of acceptable corrective action (i.e., a
statement that the lab has established blank acceptance criteria not to exceed 50% of the
reporting limit, as well as submission of benchsheets which document the new requirements)
was received by email on 3/1/2016 with an implementation date of 3/1/2016. All data reviewed
during the inspection met the required acceptance criteria. No further response is necessary
for this Finding.
Fluoride — Standard Methods, 4500 F- C-1997 (Aqueous)
pH — SW846 9045 ® (Non -Aqueous)
Phosphorus, Total —Standard Methods, 4500 P F-1999 (Aqueous)
Residue, Suspended — Standard Methods, 2540 ®-1997 (Aqueous)
Comment: The benchsheets did not document the facility name. This is considered pertinent
information. The North Carolina Administrative Code, 15A NCAC 2H .0805 (a) (7) (A) states: 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. Notification of acceptable corrective action (i.e.,
revised benchsheets including the facility name) was received by email on 3/1/2016 with an
implementation date of 3/1/2016. No further response is necessary for this Finding.
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#330 PCS Phosphate Company, Inc.
Chlorine, Total Residual — Standard Methods, 4500 Cl G-2000 (Aqueous)
Conductivity —Standard Methods, 2510 B-1997 (Aqueous)
pH — Standard Methods, 4500 H+B-2000 (Aqueous)
pH — SW846 9045 D (Non -Aqueous)
Comment: The benchsheets did not document the date and time of meter calibration. This is
considered pertinent information. The NC WW/GW Approved Procedure for the Analysis of
Specific Conductance, The NC WW/GW Approved Procedure for the Analysis of Total Residual
Chlorine, and The NC WW/GW Approved Procedure for the Analysis of pH states: The following
must be documented in indelible ink whenever sample analysis is performed: Meter calibration
and meter calibration times. Notification of acceptable corrective action (i.e., submission of
revised benchsheets including date and time of meter calibration) were received by email on
3/1/2016 with an implementation date of 3/1/2016. No further response is necessary for this
Finding.
Chlorine, Total Residual — Standard Methods, 4500 Cl G-2000 (Aqueous)
Conductivity —Standard Methods, 2510 B-1997 (Aqueous)
pH — Standard Methods, 4500 H+B-2000 (Aqueous)
pH — SW846 9045 D (Non -Aqueous)
Temperature — Standard Methods, 2550 B-2000 (Aqueous)
Comment: The benchsheets did not document the instrument IDs. The NC WW/GW Approved
Procedure for the Analysis of Specific Conductance, The NC WW/GW Approved Procedure for
the Analysis of Total Residual Chlorine, The NC WW/GW Approved Procedure for the Analysis of
Temperature and The NC WW/GW Approved Procedure for the Analysis of pH documents state:
The following must be documented in indelible ink whenever sample analysis is performed:
Instrument identification. Notification of acceptable corrective action (i.e., revised benchsheets
including the instrument IDs) was received by email on 3/1/2016 with an implementation date of
3/1/2016. No further response is necessary for this Finding.
IV. PAPER TRAIL INVESTIGATION:
The paper trail consisted of comparing original records (e.g., laboratory benchsheets, logbooks,
etc.) and contract lab reports to Discharge Monitoring Reports (DMRs) submitted to the North
Carolina Division of Water Resources. Data were reviewed for PCS Phosphate Company, Inc.
(NPDES permit # NC0003255) for July, August and September, 2015. No transcription errors
were detected. The facility appears to be doing a good job of accurately transcribing data.
V. CONCLUSIONS:
All Findings noted during the inspection were adequately addressed prior to the completion of
this report. The inspector would like to thank the staff for its assistance during the inspection and
data review process. No response is required.
Report prepared by: Nick Jones Date: March 3, 2016
Report reviewed by: Tonja Springer Date: March 4, 2016