#20_0421_FINAL

INSPECTION REPORT ROUTING SHEET
To be attached to all inspection reports in-house only.
Laboratog Cert.#:
Laboratogg Name:
Inspection Type:
Inspector Name(s):
Inspection Date:
Date Report Completed:
Date Forwarded to Reviewer:
Reviewed by:
Date Review Completed:
Cover Letter to use:
Unit Supervisor/Chemist Ill:
Date Received:
Date Forwarded to Linda:
Date Mailed:
20
PAR Laboratories,Inc.
Commercial Maintenance
Beth Swanson.Garv Francies,Dana Satterwhite
Jason Smith,Nick Jones.Tonia Springer
April 21.2015
Mav 22,2015
May 22,2015
Tonia Springer
May 26.2015
I]lnsp.Initial E lnsp.Reg.
E]lnsp.No Finding |:|lnsp.CP
|:|Corrected El lnsp.Reg.Delay
Gaw Francies V
June 3,2015
June 17,2015
i_i
cc:Ray Terhune,EPA Region 4
Wes Bell,MRO
On-Site Inspection Report
LABORATORY NAME:PAR Laboratories,Inc.
ADDRESS:Box 411483
Charlotte,NC 28273
CERTIFICATE #:20
DATE OF INSPECTION:April 21,2015
TYPE OF INSPECTION:Commercial Maintenance
AUDlTOR(S):Gary Francies,Beth Swanson,Dana Satteiwhite,Nick Jones.
Jason Smith,Tonja Springer,and Ray Terhune (US EPA Region 4)
LOCAL PERSON(S)CONTACTED:Russell Everett and Christopher Tita
I.INTRODUCTION:
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.
ll.GENERAL COMMENTS:
Ray Terhune,representing the United States Environmental Protection Agency (USEPA)Program,
Region 4,Science and Ecosystem Support Division,Office of Quality Assurance,accompanied the NC
WW/GW LC auditors on this inspection to offer support and assistance.
Proficiency Testing (PT)samples for the 2015 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 30,2015.
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 K &W Laboratories (Certification #559)and Accutest Laboratories
Southeast,Inc.(Certification #573).
Findings F,H,I,J,X,HH,and JJJ are new policies that have been implemented by our program since the
last inspection.
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FINDINGS.REQUIREMENTS,COMMENTS AND RECOMMENDATIONS:
General
Comment:The laboratory is reminded that,in accordance with 15A NCAC 2H .0805 (a)(7)(N),any time
compliance samples are received which do not meet sample collection,holding time,or preservation
requirements,the laboratory must notify the sample collector or client and secure another sample if
possible.If another sample cannot be secured,the original sample may be analyzed but the results
reported must be qualified with the nature of the infraction and the laboratory must notify our office of the
infraction.The notification must include a statement indicating corrective actions taken to prevent the
problem for future samples.No instances where notification to our office was necessary due to infractions
of this nature were observed during the inspection..
Comment:The laboratory is reminded that they can change to the current preservation and storage
temperature of s 6°C (or <10°C for bacterial tests)as stated in Code of Federal Regulations (CFR),Title
40,Part 136.3,Federal Register Vol.77,No.97,May 18,2012,Table ll.
Documentation
Comment:There were instances where the analyst’s handwriting was difficult to read,which could pose
issues with data defensibility ortranscription errors.
Recommendation:It is recommended that all nitrogen parameters be reviewed to assure that results are
documented and reported "as N”.
Recommendation:It is recommended that all records of preventative maintenance performed on
analytical instrumentation be documented in an individual equipment maintenance log book maintained
by the laboratory.All records of corrective action taken or minor troubleshooting and repair performed
should also be documented in the equipment maintenance log.The records may include the following,
as appropriate:
a.The identity of the item of equipment and its software;
b.The manufacturer’s name,type identification,and serial number or other unique
identifier;
c.The current location;
d.The dates,results and copies of reports and certificates or all calibrations,adjustments,
acceptance criteria,and the due date of the next calibration.
e.The maintenance plan,where appropriate,and maintenance completed date.
f.Documentation of any damage,malfunction,modification,or repair to the equipment.
g.Signature or initials of the person performing the maintenance or troubleshooting.
These records provide an historical reconstruction of the maintenance performed,a reference for
effective troubleshooting in the future,and can also serve as a valuable training tool for new analysts.
Recommendation:It is recommended that documentation of training and initial demonstration of
capability studies be maintained for any temporary or part-time analysts at the laboratory
Documentation of on-going demonstration of capability by these analysts is also recommended.
A.Finding:Several instances of writing over a number as a means of error correction and
corrections without initial and date were observed.
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
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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:NC WW/GW LC Policy.
Finding:The Quality Assurance Manual (QAM)must be updated.
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).'
Comment:The current QAM does not adequately reflect current laboratory practice.Submit
an updated QAM to this office by December 31,2015.
Finding:The laboratory needs to increase the documentation of purchased materials and
reagents,as well as documentation of standards and reagents prepared in the laboratory.
Requirement: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).A system (e.g.,traceable identifiers)must
be in place that links standard/reagent preparation information to analytical batches in which the
solutions are used.Documentation of solution preparation must include the analyst’s initials,
date of preparation,the volume or weight of standard(s)used,the solvent and final volume of
the solution.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.Ref:
NC V\IW/GW LC Policy.
Finding:Analysts were not always documenting the full date of analyses on 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.Ref:15A NCAC 2H .0805 (a)(7)
(H)-
Comment:Dates were often recorded as MM/DD with no year.
Finding:Units of measure were not documented in several locations.
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.Ref:15A NCAC 2H .0805 (a)(7)
(H).
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Comment:Check all benchsheets for the presence of units of measure.Examples where units of
measure were missing include:
MBAS benchsheet -initial calibration verification (ICV)
Conductivity benchsheet -calibration check values
Chloride benchsheets -units of measure are not documented
Oil &Grease benchsheets -units of measure are not documented
COD benchsheets -units of measure are not documented
BOD benchsheets —most units of measure are not documented
Quality Control
Recommendation:It is recommended that the analysis of the pH check buffer be documented on the
calibration log of the pH meter in the lab.The lab does not currently conduct pH analysis for regulatory
reporting with this meter.lt is recommended that the meter be assigned an ID and this be documented on
the calibration log.
Comment:Currently the NIST traceable reference thermometer is being recertified every year and the
weights sets are verified every 2 years.Our weight verification policy states that ASTM Class 1 and 2
weights must be verified at least every 5 years.The Calibration and Verification of Temperature Sensing
Devices policy states:NIST certified thermometers must be recalibrated,at a minimum,every five years.
A new certificate must be issued and maintained for inspection upon request.Recalibrate sooner if the
thermometer has been exposed to temperature extremes.
F.Finding:The infrared (IR)thermometer used to measure sample temperature upon receipt is not
checked daily.
Requirement:Each day of use,perform a single check of the IR thermometer by checking the
temperature of a bottle of water at the temperature of interest that contains a calibrated
thermometer.Agreement between the two must be within O.5°C,or the device must be
recalibrated.If the second calibration fails,the device must be repaired and/or replaced.
Document the quarterly and daily calibration checks.Ref:NC WW/GW LC Policy.
G.Finding:The fecal coliform water bath digital thermometer calibration is checked with an NIST
traceable reference thermometer that is graduated in increments of 1°C.
Requirement:Each laboratory requesting certification must contain or be equipped with the
following:Glassware,chemicals,supplies,and equipment required to perform all analytical
procedures included in their certification.Ref:15A NCAC 2H .0805 (a)(6)(H)
Requirement:Annually or,preferably,semiannually check accuracy of all working
temperature-sensing devices,such as liquid-in-glass thermometers,thermocouples,and
temperature recording instruments at the use temperature against a certified NIST thermometer
or one traceable to NIST and conforming to NIST specifications.Ref:Standard Methods,9020
B-2005.(4)(a).
Comment:A reference thermometer with 1°C increments is not adequate to verify the calibration
of the digital water bath thermometer which reads to 0.1°C degree increments.Due to the tight
acceptance criterion of the water bath temperature,i.e.,44.5 1 O.2°C,a O.1°C temperature sensor
is needed to maintain the proper water bath temperature.To save money,rather than purchasing
a reference NIST traceable thermometer with the necessary gradations,a new NIST traceable
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thermometer with the proper gradations could be purchased yearly to use for the water bath
thermometer calibration check.
Proficiency Testing
H.Finding:The laboratory is not analyzing Proficiency Testing (PT)samples in the same manner
as environmental samples.
Requirement:All PT samples are to be analyzed and the results reported in a manner
consistent with the routine analysis and reporting requirements of compliance samples and any
other samples analyzed according to the requirements of 15A NCAC 2H .0800.Ref:Proficiency
Testing Requirements,February 20,2012,Revision 1.2.
Comment:As an example,the laboratory’s common practice for chloride was to analyze a known
standard along with the PT sample as additional quality control.Since this is not performed with all
environmental samples,it is considered additional quality control.However,known samples are
recommended when analyzing remedial PT samples as part of the troubleshooting and corrective
action process.
I.Finding:The laboratory is not documenting PT sample analyses in the same manner as
environmental samples.
Requirement:All PT sample analyses must be recorded in the daily analysis records as for any
environmental sample.This sen/es as the permanent laboratory record.Ref:Proficiency
Testing Requirements,February 20,2012,Revision 1.2.
Comment:The analysis of PT samples is designed to evaluate the entire process used to
routinely report environmental analytical results;therefore,PT samples must be analyzed and
the process documented in the same manner as environmental samples.The laboratory is not
entering PT samples into their tracking system and PTs analyzed for parameters without clients
are written directly on the report form.
J.Finding:The preparation of PT samples is not documented.
Requirement:PT samples received as ampules must be diluted according to the PT provider’s
instructions.The preparation of PT samples must be documented in a traceable log or other
traceable format.The diluted PT sample becomes a routine environmental sample and is added
to a routine sample batch for analysis.Ref:Proficiency Testing Requirements,February 20,
2012,Revision 1.2.
Comment:For any PT samples which require preparation,dating and initialing the instruction
sheet for the preparation of the PT sample would satisfy the documentation requirement.
Standard Operating ProceduresIQuaIity Assurance Manual
Comment:Unclear verbiage is used in many SOPs regarding acceptance criteria,e.g.,“duplicates must
not vary by >10%”,that needs to be further explained or defined.Including the calculations for
determining duplicate acceptance criteria would make it clearer.
Recommendation:It is recommended that the laboratory implement a controlled SOP management
system to ensure the most up to date versions are being used by all analysts.
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Recommendation:It is recommended that all SOPs be reviewed for the use of the word “should”.For
example,in the QC section of the fecal coliform SOP,the blank criteria is listed as “should”but listed as
“must”in the procedure section.
K.Finding:All SOPs need to be reviewed and updated.The list below,while not all inclusive,states
specifics that were noted during the time of inspection:
0 The method reference in the SOP is not correct (except where noted in this report,samples
were analyzed and reported by the proper method).
o Mercury (EPA 245.1,Rev.3.0 (1994))—The SOP references EPA 245.2.
0 Total Kjeldahl Nitrogen ((SM,4500 Norg C-1997(SM 4500 NH3 G-1997))-The
SOP references EPA 351.2.
o Chloride (SM 4500 cr B-1997)-The SOP references Standard Methods 20"“
Edition rather than the year of Standard Methods Committee approval.
o COD (EPA 410.4,Rev.1.0 (1993))-The SOP does not include citation of the
reference method.
o Oil &Grease (EPA 1664 Rev.B)-The SOP does not include citation of the
reference method.
o Phenol (EPA 420.1 (Rev.1978))-The SOP references EPA 420.2.
-The SOP is in direct conflict with the method and/or a regulatory requirement.
o Metals (EPA 200.7,Rev.4.4 (1994))—The SOP states that 3mL of HNO3 is used for
digestion.The method requires 2mL of HNO3 and 1mL of HCI,which is the procedure
followed by the analyst.
o Metals (EPA 200.7,Rev.4.4 (1994))-The wavelengths listed in Table 1 of the SOP
do not match the wavelengths in the method,or the wavelengths used by the
laboratory.
-The laboratory does not have an SOP for this parameter.
o Total Dissolved Solids (SM 2540 C-1997)
-The SOP does not describe in detail how the method is performed.
o Oil &Grease (EPA 1664 Rev.B)—The SOP is a cut and paste directly from the
method.The SOP needs to state the specific procedure,QC limits,corrective action,
etc.,used.
o Metals (EPA 200.7,Rev.4.4 (1994))-The working calibration standard recipe in the
SOP does not include all the metals listed on the laboratory’s certified parameter list.
The following metals need to be added:aluminum,arsenic,iron,manganese,and
selenium.
0 Metals (EPA 200.7,Rev.4.4 (1994))-The SOP states that preservation takes place
“as soon as possible,preferably at time of collection”.It needs to state that
preservation is done either within 15 minutes or at least 24 hours prior to analysis to
ensure the preservation and hold time requirements prescribed in CFR,Title 40,Part
136.3,Federal Register Vol.77,No.97,May 18,2012,Table ll,are met.
0 Metals (EPA 200.7,Rev.4.4 (1994))-The SOP does not define the duplicate
acceptance criteria.
o Fecal Coliform (SM 9222 D-1997)-The SOP does not define the duplicate
acceptance criteria.
o Cyanide (EPA 335.4,Rev.1.0 (1993))-The SOP does not address the analysis of
matrix spikes.
o Cyanide (EPA 335.4,Rev.1.0 (1993))-The SOP does not address the analysis of
blanks.
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0 Cyanide (EPA 335.4,Rev.1.0 (1993))—The SOP does not address the minimum
correlation coefficient requirement for the calibration curve.
o Cyanide (EPA 335.4,Rev.1.0 (1993))-The SOP does not address sample
preservation.
o Fecal coliform (SM 9222 D-1997)-The SOP does not include the purchased
prepared plates in the supply list.
o All SOPs for analyses which include a calibration curve must note that any sample
results which exceed the highest concentration used in the curve must be diluted to a
concentration that is bracketed by two calibration standard concentrations of the curve.
o All SOPs must reference the QAM when there are omissions in those SOPs regarding
acceptance criteria and/or corrective actions.
~Personnel were not following procedures as stated in the Laboratory’s SOP.
o MBAS (SM 5540 C-2000)—The QAM states that the duplicate acceptance criterion
is based off Relative Percent Difference (RPD),but analysts have been using
percent error.
o COD (EPA 410.4,Rev.1.0 (1993))-Section l.E.of the SOP states that blanks are
being reused.The analyst is not doing this,so it needs to be removed from the SOP.
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).Please submit 2 updated SOPs per month with the items listed
above addressed such that all revised SOPs are submitted by December 31,2015.
Recommendation:It is recommended that SOPs include a revision and review history with
relevant dates (e.g.,effective,review and revision dates)and a brief description of the
change(s)made.
Recommendation:It is recommended that during the SOP review process,all current methods
are compared to the 40 CFR Methods Update Rule (MUR)published on May 18,2012 to make
sure the most recently approved method is being used and that all benchsheets and supporting
documentation are updated to reflect those changes.
Total Dissolved Solids -Standard Methods,2540 C-1997
Total Suspended Solids -Standard Methods,2540 D-1997
Finding:The samples are not weighed to constant weight,nor is an annual multiple weighing
study,to verify the adequacy of the drying time,performed.
Requirement:Constant weights must be documented.The approved methods require the
following:“Repeat the cycle of drying,cooling,desiccating,and weighing until a constant weight
is obtained or until the weight change is less than 4%of the previous weight or 0.5 mg,
whichever is less.”In lieu of this,an annual study documenting the time required to dry
representative samples to a constant weight may be performed.Verify minimum daily drying
time is greater than or equal to the time used for the initial verification study drying cycle.Drying
cycles must be a minimum 1 hour for verification.Ref:NC WW/GW LC Policy.
Comment:North Carolina allows for an annual drying study in lieu of the requirement above to
repeat the drying cycle for every sample.A random full set of samples should be used for the
drying study.The repeated drying time in the oven should be at least 1 hour long.The time
used for the annual drying study is the minimum time that samples are to be dried until a new
drying study is performed.
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Total Suspended Solids —Standard Methods,2540 D-1997
M.Finding:The laboratory is not basing the reporting limit on the volume of sample used.
Requirement:The minimum weight gain allowed by any approved method is 2.5 mg.Choose
sample volume to yield between 2.5 and 200 mg dried residue.This establishes a minimum
reporting value of 2.5 mg/L when 1000 mL of sample is analyzed.If complete filtration takes
more than 10 minutes increase filter diameter or decrease sample volume.In instances where
the weight gain is less than the required 2.5 mg,the value must be reported as less than the
gppropriate value based upon the volume used.Ref:NC WW/GW LC Policy.
Comment:The lab is using a static reporting limit of 5 mg/L.The reporting limit is 5 mg/L only
when 500mL of sample is used.When taking into account the method required 2.5 mg weight
gain and the volume of sample used,the reporting limit is calculated using the following
equation:RL=(2.5mg/vol used in mL)*1000.
Ammonia as N -EPA 350.1,Rev 2.0 (1993)
Nitrate +Nitrite as N —EPA 353.2,Rev.2.0 (1993)
N.Finding:A Laboratory Reagent Blank (LRB)is not being analyzed as required by the methods.
Requirement:The laboratory must analyze at least one LRB with each batch of samples.Ref:
EPA Method 350.1,Rev.2.0 (1993),Section 9.3.1.
Requirement:The laboratory must analyze at least one LRB with each batch of samples.Ref:
EPA Method 353.2,Rev.2.0 (1993),Section 9.3.1.
Recommendation:It is recommended that all parameters be evaluated to determine if
LRBs/method blanks/preparation blanks are required per the applicable methods.
Ammonia as N -EPA 350.1,Rev.2.0 (1993)
Recommendation:It is recommended that the quarterly distillation study be more representative of
the client types for which ammonia samples are analyzed,i.e.,include more industrial samples.The
Ammonia/Fluoride Distillation Studies Policy states:Commercial Laboratories shall analyze initially 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 wastes types.
Total Kieldahl Nitrogen as N —Standard Methods,4500 Norg C-1997 (Standard Methods,4500
NH3 G-1997)
Total Phosphorous —EPA 365.3 (Issued 1978)
O.Finding:The analyst is recording the dilution factor in the column labeled “pH<2”.
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 volume to be reported and
each item must be recorded each time samples are analyzed.Ref:15A NCAC 2H .0805 (a)(7)
(H).
Comment:Recording information under incorrectly labelled headers could compromise data
defensibility.
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Total Kieldahl Nitrogen as N —Standard Methods,4500 Norg C-1997(Standard Methods,4500
NH3 G-1997)
Recommendation:It is recommended that copper sulfate be used as the catalyst in place of mercuric
sulfate as allowed by footnote 5 in Table IB of 40 CFR Part 136.3.
}m —Standard Methods,4500 H+B-2000
Comment:An Automatic Temperature Compensation (ATC)check is not required for pH meters.
P.Finding:Calibration of the pH meter used in the field for compliance monitoring is not
documented.
Requirement:The following must be documented in indelible ink whenever sample analysis is
performed.Meter calibration,meter calibration time(s),true value of buffers used for calibration,
true value for the check standard buffer,and value obtained for the check standard buffer
(verification of i 0.1 Standard Units (S.U.)).Ref:NC \/\/IN/GW LC Approved Procedure for the
Analysis of pH.
Recommendation:It is recommended that a supplemental or separate field pH SOP be
developed.A copy of the NC WW/GW LC Approved Procedure for the Analysis of pH was
provided at the time of the inspection.
Cyanide —EPA 335.4,Rev.1.0 (1993)
Comment:The lab is currently having samples preserved to pH greater than 12 s.u.but samples may be
preserved to pH greater than 10 s.u.as required in 40 CFR 136.3 Table ll.
Recommendation:It is recommended that the graphical depiction of calibration curves be printed for
quality control evaluation.
Recommendation:It is recommended that it is documented in the SOP that the flags reported from the
measurement system are legacy and not used.
Recommendation:It is recommended that cyanide distillations be conducted under a fume hood.
Recommendation:It is recommended that the laboratory purchase Standard Practice for Sampling,
Presen/ation and Mitigating interferences in Water Samples for Analysis of Cyanide,ASTM D7365-09a.
Q.Finding:The laboratory is not calculating and documenting the percent recovery of the
calibration verification and/or laboratory control standards on the benchsheet.The laboratory is
not documenting the duplicate acceptance criterion on the benchsheet.
Requirement:The quality control results obtained must be documented on the benchsheet and
evaluated against established acceptance criteria to demonstrate that the analyst was aware of
any out-of-control situation.The corrective actions taken must be documented.Any samples
not meeting the acceptance criteria must be reanalyzed,if possible.If this is not possible,the
data must be flagged on the laboratory reports and Discharge Monitoring Reports (DMRs)as all
quality control requirements not met.Ref:15A NCAC 2H .0805 (a)(7)and 15A NCAC 2H .0805
(8)(F)-
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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).
R.Finding:Samples and standards do not appear to be distilled before analysis.
Requirement:Manual distillation with MgCl2,followed by any of the following:Semi-Automated.
Ref:CFR,Title 40,Part 136.3;Federal Register Vol.77,No.97,May 18,2012;Table IB.
Comment:It is not required that all standards be distilled in the same manner as the samples.It
is recommended that at least two standards (a high and low)and a blank be distilled and
compared to similar values on the standard curve to insure that the distillation technique is
reliable.If distilled standards do not agree within :10%of the undistilled standards the analyst
should find the cause of the apparent error before proceeding.Before distillation,standards
should contain 4 mL 0.25N NaOH per 50 mL.
S.Finding:The process of checking samples for sulfides and nitrates/nitrites before analysis was
not documented.
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:15 NCAC 2H .0805 (a)(7)
(A).
T.Finding:The dilution factor for each sample is not documented on the benchsheet.
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 volume to be
reported and each item must be recorded each time samples are analyzed.Ref:15A NCAC 2H
.0805 (a)(7)(H).
Phenol —EPA 420.1 (Rev.1978)
Total Phosphorous -EPA 365.3 (Issued 1978)
U.Finding:The laboratory is referencing a no longer approved method on the benchsheets and
client reports.
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:15 NCAC 2H .0805 (a)(7)
(A)-
Comment:For phenol,the benchsheets and client reports reference EPA 420.2,which is no
longer an EPA approved method.For total phosphorous,the benchsheet and SOP reference
EPA 365.2 and the client reports and digestion log reference EPA 365.4,which are all no longer
approved methods.
Phenol -EPA 420.1 (Rev.1978)
Comment:At the time of the inspection,the laboratory’s certified parameter list did not include phenol.
Upon review,it was determined that the laboratory requested it to be included on their certified
parameter list during the application update,requested by NC \/VW/GW LC,after the 2012 Method
Update Rule.The parameter was inadvertently left off the certified parameter list.The lab has analyzed
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acceptable PTs for this parameter since that time and was under the impression that they were
certified.Acceptable corrective action (i.e.,Phenol EPA 420.1,Rev.1978 was added to the certified
parameter list with an effective date of January 1,2015)was implemented on May 18,2015.No
response is necessary for this finding.
V.Finding:The analyst is not documenting the stock standardization.
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).
Recommendation:It is recommended that a stock standardization worksheet be developed
and used.
Sulfide —Standard Methods,4500 S2‘F-2000
W.Finding:The laboratory is analyzing and reporting data by a method not approved by the EPA,
i.e.,Standard Methods 4500 s2"E.
Requirement:Analytical methods,sample preservation,sample containers and sample holding
times shall all conform to those requirements found in 40 CFR-136.3.Ref:15A NCAC 2H .0805
(a)(1)-
Metals —EPA 200.7,Rev.4.4 (1994)
Recommendation:According to section 9.2.4 of the method,it is recommended that a method detection
limit (MDL)study be performed when a new analyst begins work,annually,and when a change in
analytical performance caused by a change in instrument hardware or operating conditions occur.
X.Finding:The volume of spike solution used in matrix spike preparation exceeds 10%of the
total matrix spike volume.
Requirement:The volume of spike solution used in matrix spike preparation must in all cases
be s 10%of the total matrix spike volume.It is preferable that the spike solution constitutes s
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
adjusted by calculation.Ref:NC WW/GW LC Policy.
Y.Finding:The digestion is not properly performed.
Requirement:Reduce the volume of the sample aliquot to about 20 mL by gentle heating at
85°C.DO NOT BOIL.This step takes about two hours for a 100 mL aliquot with the rate of
evaporation rapidly increasing as the sample volume approaches 20 mL.(A spare beaker
containing 20 mL of water can be used as a gauge.)11.2.5 Cover the lip of the beaker with a
watch glass to reduce additional evaporation and gently reflux the sample for 30 minutes.
(Slight boiling may occur,but vigorous boiling must be avoided to prevent loss of the HCI-H O
azeotrope.)Ref:EPA method 200.7,Rev.4.4 (1994),Sections 11.2.4 and 11.2.5.
Comment:The analyst currently digests to near dryness and does not reflux with the sample
covered to prevent additional evaporation.
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Finding:A calibration blank is not analyzed initially,after every 10 samples,and at the end of
analysis.
Requirement:The calibration blank and calibration verification standard (mid-range)must be
analyzed Il'lIIIaIIY_(I.€.,J)l'I0l'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.).Ref:NC WW/GW LC Policy.
Comment:The calibration blank does not require digestion.
Finding:The laboratory is not using the method required acceptance criteria for the instrument
performance check analyzed immediately following calibration.
Requirement:Analysis of the IPC solution immediately following calibration must verify that the
instrument is within 15%of calibration with a relative standard deviation <3%from replicate
integrations 24.Ref:EPA method 200.7,Rev.4.4 (1994),Section 9.3.4.
Finding:The second source quality control standard (QCS)acceptance criterion is greater than
the method required i 5%.
Requirement:Quality control sample (QCS)-When beginning the use of this method,on a
quarterly basis,after the preparation of stock or calibration standard solutions or as required to
meet data-quality needs,verify the calibration standards and acceptable instrument performance
with the preparation and analyses of a QCS (Section 7.12).To verify the calibration standards the
determined mean concentrations from three analyses of the QCS must be within 15%of the
stated values.If the calibration standard cannot be verified,performance of the determinative step
of the method is unacceptable.The source of the problem must be identified and corrected before
either proceeding on with the initial determination of method detection limits or continuing with on-
going analyses.Ref:EPA Method 200.7,Rev.4.4 (1994),Section 9.2.3.
Total Phosphorous -EPA 365.3 (Issued 1978)
MBAS -Standard Methods,5540 C-2000
CC.
DD.
Finding:The benchsheets do not include the acceptance criteria for quality control elements.
Requirement:The qualitv control results obtained must be documented on the benchsheet
and evaluated against established acceptance criteria to demonstrate that the analyst was
aware of any out-of-control situation.The corrective actions taken must be documented.Any
samples not meeting the acceptance criteria must be reanalyzed,if possible.If this is not
possible,the data must be flagged on the laboratory reports and Discharge Monitoring Reports
(DMRs)as all quality control requirements not met.Ref:15A NCAC 2H .0805 (a)(7)and 15A
NCAC 2H .0805 (a)(F).
Finding:The benchsheets do not show the calculation of the duplicate and standard recoveries.
Requirement:The quality control results obtained must be documented on the benchsheet and
evaluated against established acceptance criteria to demonstrate that the analyst was aware of
any out-of-control situation.The corrective actions taken must be documented.Any samples
not meeting the acceptance criteria must be reanalyzed,if possible.If this is not possible,the
data must be flagged on the laboratory reports and Discharge Monitoring Reports (DMRs)as all
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quality control requirements not met.Ref:15A NCAC 2H .0805 (a)(7)and 15A NCAC 2H .0805
(8)(F)-
MBAS -Standard Methods,5540 C-2000
Recommendation:It is recommended that the peroxide treatment,as stated in section (4)(c)of the
method for sulfide interference,be added to the SOP in case sulfide mitigation is ever needed.
Recommendation:It is recommended that the benchsheet be updated to include the approved method
reference year with the method citation.
EE.Finding:The correlation coefficient of the curve is not documented.The correlation coefficient is
considered pertinent data.
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:15 NCAC 2H .0805 (a)(7)
(A).
FF.Finding:Sample results are not reported in terms of linear alkylbenzene sulfonate (LAS)
molecular weight.
Requirement:Report as “MBAS,calculated as LAS,mol wt Ref:Standard Methods,
5540 C-2000.(5).
GG.Finding:The curve does not specify the molecular weight of the LAS used.
Requirement:Treat each standard as described in 1js 4d and e following,and plot a calibration
cun/e of absorbance vs.micrograms LAS taken,specifying the molecular weight of LAS used.
Ref:Standard Methods,5540 C-2000.(4)(a).
HH.Finding:The laboratory is not analyzing matrix spikes.
Requirement: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 each month samples are analyzed.Prepare the matrix spike from a
reference source different from that used for calibration unless othen/vise stated in the method.
If matrix spike 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 matrix spike 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.Ref:NC WW/GW LC Policy.
Comment:The matrix spike may be analyzed as a matrix spike/matrix spike duplicate to meet
both the spiking and duplication requirements.
Cyanide —EPA 335.4,Rev.1.0 (1993)
MBAS —Standard Methods,5540 C-2000
Total Phosphorous —EPA 365.3 (Issued 1978)
ll.Finding:The preparation of standards is not documented in such a way as to provide
traceability between standards and their use during analyses.
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Requirement: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).A system (egg,traceable identifiers)must
be in place that links standard/reagent preparation information to analytical batches in which the
solutions are used.Documentation of solution preparation must include the analyst’s initials,
date of preparation.the volume or weight of standard(_s)used.the solvent and final volume of
the solution.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.Ref:
NC WW/GW LC Policy.
Comment:The laboratory must provide an adequate means,through log books and/or
electronically,to ensure a standard used in analysis can also be traced to a certified vendor or
NEAT lot.
Conductivity -EPA 120.1 (Rev.1982)
Comment:Since it is a field parameter,the analysis of duplicate samples is not required for conductivity.
Comment:After calibration,only one calibration check standard is required.
JJ.
KK.
LL.
Finding:Calibration checks were incorrectly labeled as calibration standards on the benchsheet.
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:15 NCAC 2H .0805 (a)(7)
(A)-
Finding:Quality control elements that are analyzed are not evaluated to assure they meet
acceptance criteria.
Requirement:The quality control results obtained must be documented on the benchsheet and
evaluated against established acceptance criteria to demonstrate that the analyst was aware of
any out-of-control situation.The corrective actions taken must be documented.Any samples
not meeting the acceptance criteria must be reanalyzed,if possible.If this is not possible,the
data must be flagged on the laboratory reports and Discharge Monitoring Reports (DMRs)as all
quality control requirements not met.Ref:15A NCAC 2H .0805 (a)(7)and 15A NCAC 2H .0805
(a)(F)-
Finding:Results are reported as “umhos/cm”,not the method required “umhos/cm at 25°C".
Requirement:Report results as Specific Conductance,umhos/cm at 25°C.Ref:EPA Method
120.1,(Rev.1982),Section 9.2.
Chloride —Standard Methods,4500 Cl‘B-1997
MM.Finding:The spreadsheet is miscalculating the results.
Requirement:Standard silver nitrate titrant,0.0141M (0.0141N).Ref:Standard Methods 4500
Cl"B-1997.(3)(b).
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Requirement:As a starting point,round off the results of any calculation in which several
numbers are multiplied and divided to as few significant figures as are present in the factor with
the fewest significant figures.Ref:Standard Methods 1050 B-2006.(5).
Comment:The excel spreadsheet used to calculate results uses a normality for the silver nitrate
titrant with 16 decimal places instead of 4.The spreadsheet was put into use around 2011 and
calculates results that are artificially high.For example,on 3/31/15,results should have been
328.82 mg/L instead of 338.88 mg/L.
Recommendation:It is recommended that the laboratory perform diagnostic testing of
spreadsheets each day they are used to generate data.This is very important where
spreadsheets or formula cells are not protected.This may be performed by entering a test
concentration in a random cell that should produce a known theoretical value
Finding:Original records are not complete.
Requirement:Supporting records shall be maintained as evidence that these practices are being
effectively carried out.All analytical records must be available for a period of five years.Ref:15A
NCAC 2H .0805 (a)(7)and (a)(7)(G).
Comment:In some instances,the analysis of a duplicate sample is written on the results
benchsheet but does not appear on the original benchsheet.This was specifically noted on data
from 3/30/15 and 8/26/14.
Finding:Neither a laboratory fortified matrix (LFM)nor a laboratory fortified matrix duplicate
(LFMD)are being analyzed.
Requirement:Include at least one LFM/LFMD daily or with each batch of 20 or fewer samples.
Ref:SM 4020 B-2009,Table 4020:l and (2)(g).
Comment:Since an LFM and LFMD are required by the method,this satisfies the NC \/VW/GW
LC duplicate requirement.
Finding:Compliance data is indistinguishable from other data.
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:15 NCAC 2H .0805 (a)(7)
(A)-
Comment:The analyst stated that “NSR”,which stands for “non state reported”data,was written
on benchsheets which contained data that was not for state reporting.No sheets were found with
this acronym.
Recommendation:It is recommended that a statement explaining “NSR”be added to the
laboratory’s QAM.
Finding:There were instances of incorrect or incomplete dates on 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.Ref:15A NCAC 2H .0805 (a)(7)
(H)-
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Comment:Some of the secondary benchsheets had the wrong year in the page header and no
year next to the initial and date.
COD -EPA 410.4,Rev.1.0 (1993)
RR.Finding:The laboratory is not analyzing matrix spikes.
Requirement:Laboratory Fortified Sample Matrix (LFM)-The laboratory must add a known
amount of analyte to a minimum of 10%of the routine samples.Ref:EPA 410.4,Rev.1.0 (1993),
Section 9.4.1.,
Oil &Grease -EPA 1664 Rev.B
SS.Finding:The PQL is not being adjusted when less than 1L of sample is being analyzed.
Requirement:Determine the original sample volume (Vs)in liters by filling the sample bottle to
the mark with water and measuring the volume of water in a 1-to 2-L graduated cylinder.If the
sample weight was used (Section 11.1.4),weigh the empty bottle and cap and determine Vs by
difference,assuming a sample density of 1.00.Ref:EPA method 1664 Rev.B,Section 11.4.5.
Requirement:n-Hexane extractable material —Calculate the concentration of HEM (“oil and
grease”)in the sample per the following equation:HEM (mg/L)=(Wh in mg)/(Vs in L)
where:
Wh =Weight of extractable material from Section 11.4.4.1 (mg)
Vs =Sample volume from Section 11.4.5 (L).
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Ref:EPA method 1664 Rev.B,Section 12.1.I
Fecal Coliform —Standard Methods,9222 D-1997
IRecommendation:It is recommended that the laboratory begin performing monthly colony verifications I
as outlined in Standard Methods 9222 D-1997.(2)(f).I
Comment:For sample duplicates,only one dilution per sample is required to be duplicated.
Recommendation:It is recommended that the benchsheet be updated to include the year of the
currently approved reference method.
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TT.Finding:The laboratory is not monitoring the quality of the reagent water used for fecal coliform
analysis.
Requirement:Fecal coliform reagent water must be analyzed every twelve months to ensure I
suitability.At a minimum analyses must be performed for conductivity,TOC,Cd,Cr,Cu,Pb,and .
Zn.Recommended limits for reagent water quality are given in Standard Methods 9020 B-2005
Table 9020:ll.If these limits are not met,investigate and correct or change water source.Ref:NC
WW/GW LC Policy and Standard Methods 9020 B-2005.(5)(f).
UU.Finding:Heat-indicating tape is not used with all materials each sterilizing cycle.
Requirement:Use heat-indicating tape to identify supplies and materials that have been
sterilized.Ref:Standard Methods 9020 B-2005.(4)(h).
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VV.
WW.
XX.
YY.
ZZ.
AAA.
Finding:The laboratory is not documenting the items sterilized and the operating parameters of
the pressure cooker during each sterilization cycle.
Requirement:Record items sterilized and sterilization temperature along with total run-time
(exposure to heat),actual time period at sterilization temperature,set and actual pressure
readings,and initials of responsible person for each cycle.Ref:Standard Methods 9020 B-2005.
(4)(II)-
Finding:The laboratory is not consistently using an approved technique to sterilize the filtration
apparatus.
Requirement:Wrap the assembly (as a whole or separate parts)in heavy wrapping paper or
aluminum foil,sterilize by autoclaving and store until use.Ref:Standard Methods 9222 B-1997.
(1)(f).Referenced in Standard Methods 9222 D-1997.(2)(b).
Comment:The funnels were sterilized using alcohol.
Finding:The time that the sample is filtered is not recorded on the benchsheet to show that no
more than 30 minutes has passed before filters are placed into the incubator.
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:15 NCAC 2H .0805 (a)(7)
(A)-
Requirement:Place all prepared cultures in the water bath within 30 min after filtration.Ref:
Standard Methods 9222 D-1997.(2)(d).
Finding:Incubator temperature is only checked one time per day.
Requirement:When incubator is in use,monitor and record calibration-corrected temperature
twice daily.Ref:Standard Methods,9020 B-2005.(4)(n).
Finding:Duplicate filters are not being included in the result calculation.
Requirement:The results of all tests on the characteristics of the effluent,including but not
limited to NPDES permit monitoring requirements,shall be reported on the monthly report forms.
Ref:15A NCAC 2B .0506 (b)(3)(J).
Finding:Fecal colony counts are not being properly reported in instances where there are no 100
mL dilutions and multiple membranes not within ideal range.
Requirement:Countable Membranes with less than 20 Blue Colonies:If all counts are below the
lower limit (20)of the ideal counting range:
(a)Select the count most nearly acceptable and compute the count using the general
formula.Report the count as an Estimated Count per 100 ml:gr
(b)Total the counts on all filters and report as number per 100 ml.Ref:NC WW/GW LC
Policy
Comment:For example,the benchsheet from 1/12/2015 documented a sample with a 50 mL
dilution that had 16 colonies and a 10mL dilution that had 10 colonies.The sample was reported
as 16 colonies per 100 mL,but it should have been reported as:((16 +10)counts *100)/(50 +10)
mL =43 colonies per 100 mL.
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BBB.
CCC
DDD
Finding:Purchased prepared plates used for the Fecal Coliform MF method are not properly
tested before being put into use.
Requirement:When a new lot of culture medium,pads,or membrane filters is to be used,a
comparison of the current lot in use (reference lot)against the new lot (test lot),be made.As a
minimum,make single analyses on five positive samples.Ref:NC WW/GW LC Policy.
Comment:At the time of inspection,there were only 4 plates available of the reference lot and a
consumables test had not yet been completed on the new lot.Submit documentation of the
consumable test that was performed on these four plates and subsequent testing of the
next lot of plates with the inspection response.
Recommendation:It is recommended that new consumables be tested as soon as possible
after receipt to avoid problems if the materials are not acceptable.Once you determine that the
new material is acceptable to use;you may begin to do so.Document the date the new lot
number is put into use.
Finding:There is no traceability documented for the purchased prepared plates.
Requirement: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).Consumable materials such as pH
buffers,lots of pre-made standards and/or media,solids and bacteria filters.etc.are included in
this requirement.Ref:NC \/\/IN/GW LC Policy.
Comment:Retaining the sticker applied to each sleeve of plates,along with the certificate of
analysis,will supply the required traceability.
Finding:The purchased prepared plates in use at the time of inspection were expired.
Requirement:Adherence to manufacturer expiration dates is required.Chemicalslreagentsl
consumables exceeding the expiration date can no longer be considered reliable.If the expiration
is only listed as a month and year (with no specific day of the month),the last day of the month
will be considered the actual date of expiration.Monitor materials for changes in appearance or
consistency.Any changes may indicate potential contamination and the item should be
discarded,even if the expiration date is not exceeded.If no expiration date is given,the laboratory
must have a policy for assigning an expiration date.If no date received or expiration date can be
determined,the item should be discarded.Ref:NC WW/GW LC Policy.
Comment:The expiration date of the plates in use at the time of inspection is unknown since the
documentation stating the expiration date was not retained.It appears that the manufacturer sets
a 3 month expiration date from the time the plate was poured.The expiration date is shown on a
sticker that is applied to each sleeve of plates.The current lot of plates has been used since
approximately September,2014.
BODICBOD —Standard Methods,5210 B-2001 (Hach 10360-2011,Rev.1.2)(LDO)
EEE.
FFF.
Finding:The analyst is not adding inhibitor to the seed controls for CBOD analysis.
Requirement:Determine BOD of seed suspension as for any other sample.Ref:Standard
Methods,5210 B-2001.(6)(d).
Finding:Three dilutions of each sample are not being analyzed.
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Requirement:Using the dilution water prepared as in 1]5a,make at least three dilutions of
prepared sample estimated to produce a residual DO of at least 1.0 mg/L and a DO uptake of
at least 2.0 mg/L after 5-d incubation.Five dilutions are recommended if experience with a
particular sample does not produce at least three bottles having acceptable minimum DO
depletions and residual limits (11 6a).Ref:Standard Methods,5210 B-2001.(5)(c).
Comment:The analyst is currently setting two dilutions per sample.
GGG.Finding:Three glucose-glutamic acid (GGA)standard solutions are not being analyzed.
Requirement:Add sufficient amounts of standard glucose-glutamic acid solution (‘lj 3h)to give
3.0 mg glucose/L and 3.0 mg glutamic acid/L in each of three test bottles (20 mL GGA
solution/L seeded dilution water or 6.0 mL/300-mL bottle).The resulting average BOD for the
three bottles,after correction for dilution and seeding,must fall into the range of 198 i 30.5
mg/L.Ref:Standard Methods,5210 B-2001.(6)(b).
Comment:The analyst is currently analyzing two GGA standards.
HHH.Finding:Samples were not properly adjusted for pH.
Requirement:Check pH;if it is not between 6.0 and 8.0,adjust sample temperature to 20 1 3
°C,then ad'|ust pH to 7.0 to 7.2 using a solution of sulfuric acid or sodium hydroxide of such
strength that the quantity of reagent does not dilute the sample by more than 0.5%.The pH of
dilution water should not be affected by the lowest sample dilution.Always seed samples that
have been pH adjusted.Ref:Standard Methods,5210 B-2001.(4)(b)(1).
Comment:If adjustment was needed,the analyst was adjusting to 6.5 to 7.5 s.u.
lll.Finding:The original pH value of the sample and the adjusted pH value are not documented.
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).
JJJ.Finding:The lab is utilizing Total Residual Chlorine (TRC)indicator strips to verify the
presence/absence of TRC.
Requirement:lt 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:NC \/\IW/GW LC Policy.
Vector Attraction Reduction (VAR)
KKK.Finding:The laboratory is analyzing samples and reporting data 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 2H .0804 (a).
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Comment:There appeared to be confusion on whether we certify for the VAR options,however
an email was sent to the laboratory on March 4,2015 stating which options we certify for and
included an amendment to the application form for the laboratory to use in order to request
addition of the parameter.There was no follow through by the laboratory after that point.Until NC
W\N/GW LC certification is obtained the data must be reported as “uncertified data".
PAPER TRAIL INVESTIGATION:
The paper trail consisted of comparing original records (e.g.,laboratory benchsheets,logbooks,etc.)
chain of custodies and client reports.Data were reviewed for the following project numbers LL117306
(1/12/15),LOW117439 (1/22/15),LOW118096 (3/16/2015)and Pharr Yarns,lnc.sample 6940.No
transcription errors were detected.The facility appears to be doing a good job of accurately
transcribing data.
CONCLUSIONS:
Mr.Terhune submitted a separate audit report to the NC WW/GW LC office,which is attached at the end
of this inspection report.Where appropriate,the findings from Mr.Terhune’s report have been integrated
with those from the NC VV\N/GW LC.While we recommend taking into consideration the comments and
recommendations by Mr.Terhune,only the lettered findings in this report must be addressed as stated
below.
Correcting the above-cited findings and implementing the recommendations will help this lab to produce
quality data and meet certification requirements.The inspectors would like to thank the staff for its
assistance during the inspection and data review process.Please respond to all findings and include
an implementation date for each corrective action.
Report prepared by:Beth Swanson Date:May 22,2015
Report reviewed by:Tonja Springer Date:May 26,2015
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United States Environmental Protection Agency
.Region 4
I Science and Ecosystem Support Division
980 College Station Road
Athens,Georgia 30605-2.720
I offien ST4Q‘Zs-
“OH/IN as5'. a O/"4GENc:{Q
4"“4¢Pa0'YI‘c'¢
I.SESD Office of Quality Assurance Laboratory Audit
Report
PAR Laboratories
2217 Graham Park Drive
Charlotte,NC 28273
I Audit Conducted April 21,2015
Requestorlwoject Leader:Dana Setterwhite
,NC WW/GW Laboratory Certification Branch,Raleigh,North Carolina
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FINAL LABORATORY AUDIT REPORT
Laboratow Assessor:
5/R Y/L5’
Ray T hone,Chemist I Date I
Office of Quality Assurance
USEPA Region 4,Athens,Georgia
“II ‘run
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_.4_zLzLé_p44.A._-.Assésss-~e—~;_44%~A
\E \-_5“l_§1_i-1=‘\‘;___/”
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‘(E5 "
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
REGION 4
Science and Ecosystem Support Division
980 Collage Station Road
Athens,Georgia 30605-2720
PAR Laboratory
Assessment
Location:2217 Graham ?ark Drive,Charlotte,NC 28273
Date:April 21,2015
Assessor:Ray Terhune,Chemist
Per a request from the North Carolina We stewater/Ground Water Laboratory Certification Branch,a
Laboratory Oversight Assessment oi‘PAR Laboratory was conducted on April 2i,2015 for various
analyses performed for the National Pollution and Discharge Elimination System (NPDES)Program,by
Roy Terhune,representing the United Slates Environmental Protection Agency (USEPA),Region 4.
Science and Ecosystem Support Division (SESD),Oflico ol‘Qualiiy Assurance.
The facility laboratory had sufficient laboratory space for the analytical Instrumentation.The Laboratory
personnel was extremely limited however,for pcrfommnce tho analyses of interest.Only one analyst was
on staff for all the analyses with o part time student on cull for critical holding time analyses.
The PAR Lboralory stoffwero briefed in an opening meeting on the moming ofAprll 21,2015 where
the agenda of the assessment schedule:was provided by the North Carolina Wastewaior Assessment
Team.
Laboratory Assessment
Duo Io unusual circumstances involving this laboratory,North Carolina Wosreivatcrifimmrd Water
Laboratory Certification Branch (NC WWIGW LCB)requested a presence by USEPA to provide Federal
support during the assessment.Therefore,working in an oversight and supportive role,the USEPA
assessor has dciniled any findings,recommendations and/or comments in tho following sections.
Assessment Findings and Recommendations
F'.;:pI2 J3 GI I}
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‘Tho EPA assessor performed an overview of the laboratory processes from sample log-in through sample
dta reporting.This inspection was designed to review the overall processes of the laboratory’s sample
handling,sample analysis and report generation.An in»depth assessment of the procedures and methods
nalyzodby the laboratory was performed by the NC WWrGW LCB assessment learn.Findings
discovered during the assessment by USEPA or North Carolina will require corrective actions to be
submitted which provide satisfactory means to resolve associated issues.Corrective actions are not
required for recornmendatlnns submitted by USEPA.However,the implementation ofthe
recommendation would entrance the quality and security of the data being generated for the laboratory's
clients.
General Q,,,,,p_m,ments
The Laboratory’s personnel were very transparent in their responses with no attempts to provide false,
inppropriate or misleading infomration.The laboratory’s personnel were extremely helpful and answered
truthfully when asked about the procedures and reporting aspects of the laboratory’s normal routines.This
was a critical aspect of the oversight and indicated that any past history with PAR Laboratory has been
alleviated with excellent cooperation during the assessment.
cannot Findings
l.The Laboratory did not have good documentation of calibration standard preparation for most of
the methods assessed.The Laboratory should have log books that provide sample preparation
information (date ol‘preparation,preparation analyst's initials,standard lot numbers for
traceability,dilution details,final concentrations,etc)for each standard prepared for each
analysis.
2.Standard Operating Procedures (SOPs)were not up to date.Several procedures were not detailed
enough to provide a new analyst with the infonnation necessary to perform the analysis without
assistance.These SOPs should be updated immediately to reflect the procedural steps for each
analysis.
3.Method/Preparation blanks were not analyzed for most analyses.Most methods require some type
of procedural blank standard that verifies that the laboratory did not contaminate the samples with
compounds of interest during the sampling/analytical procedures.
4.Standard and Reagent traceability to certified vendor lots within the laboratory for all methods
and procedures was not acceptable.The laboratory should provide an adequate means,through
log books andlor electronically,to ensure a standard used in an analysis can be traced to a
cortiiied vendor or NEAT lot.
5.It must be noted in all analysis SOPs that include a calibration curve,that any sample results
which exceed the highest concentration used in the curve must be diluted to a concentration that
is bracketed by two calibration standard concentrations of the curve.
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6.Method Detection Limit studies were not available for many of the analysis procedures.This ls an
annual or semi-annual (depending on the method)requirement and also as part of 40 CFR l36.7’s
QC minimum requirements.
General Recommendations
It is highly recommended that a second analyst be brought on staff that can cover for the current analyst
in case of an emergency.It‘the Laboratory analyst is unable to perform analyses for any length of time the
Laboratory would not be able to maintain holding time requirements on many oftho analyses.The
Laboratory currently enlists the help ofa student in the area for critical holding time analyses,but this is
inadequate for the vast majority of analyses performed by the Laboratory and the part time analyst should
have documentation of an initial demonstration of capabilities for any analysis performed.
Method Specific Findings
The following are findings noted by the USEPA assessor during the oversight assessment of this
Laboratory.Please note that the assessor was in an advisory role and relinquished the majority of the
analysis assessments to the NC WW/GW LBC personnel.The limited number of analysts (one)in the
laboratory greatly reduced the ability of the assessors to properly interview for each oi‘the methods in a
timely manner,therefore the vast majority ofthe analyses and procedures were assessed by the State
Assessment Team.
Total Cyanide {EPA Method 335.4,r _l.0}
I .‘The laboratory indicated that the samples were checked for sulfides and nitrates/nitrites (to verify
proper preservation)before analysis but this was not documented.Any procedure or test
performed by laboratory personnel must be documented to verify completion.
2.Samples and standards do not appear to be distilled before analysis.Tl'u's is a requirement of the
method.This process must be included in the analysis of samples for total cyanide.
Ammonia (EPA,.method 350.1_),,_'lfotol lQield;ahl_Nitrogen_(S.tandard Method 4:100 NW C,rl 997),
Nitrate/Nitrite [EPA method 353.Q
Note the findings for these procedures were covered under the “General Findings“section of this report.
Conclusions
As noted above,the USEPA,Region 4 Office of Quality Assurance auditor's role in this assessment was
to provide oversight for a difficult situation.The Laboratory personnel were very cooperative in providing
any requested infonnation and also in answering nyquestions conceming their operation.There were n
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large number of findings noted by the NC WWRGW LCB assessment team,but most,lfnot all,could be
corrected with appropriate corrective actions.There was no indication of any fraudulent or inappropriate
activities noted during this assessment.
The North Carolina Wastewaler/Ground water Laboratory Cenification Branch assessment team is to be
commended for their professionalism,speed and thoroughness during this assessment.
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#20 PAR Laboratories,inc.
North Carolina Wastewater/Groundwater Laboratory Certification
Matrix Spiking Policy and Technical Assistance (05111/201 2)
Policy Statement
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 taka corrcctivo action to rcctify tho affect,usc anothar mcthod,or smploy tho rnathod of
standard additions.When the method of choice specifies MS performance acceptance criteria for
accuracy.and the laboratory chooses to develop statistically valid.iaboratorwspeoilic limits,the
laboratory-generated limits cannot be lass stringent than the criteria stated in the approved method.
When spiking with multl-component standards,if the method does not specify the spiking components,
the Laboratory Control Spike (LCS)and MS must contain all analyies that are reported.
If the unsplked 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 s 10%of the total MS volume.it
is preferable that the spike solution constitutes s 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.
Technical Assistance
Spike Preparation
The spike concentration may be set at either 5 to 50 times the Method Detection Limit (as determined by
the Method Detection Limit or MDL study)for the analyte,or at 1 to 1D times the ambient level [average
concentration)of tho analyte in samples.Thcrc arc ssvaral options for preparing spikes.for cxarnpic:
Option 1 (Recommended -easiest)-if the spike solution volume is equal to 1%or less of the
total sample voluma,direct subtraction of the unspiked sample is allowd.When the volume of
the standard solution spiked into a sample or a sample extract is less than 1%of the total volume
then the final concentration need not be adjusted (e.g.,10 pL of spike solution added to a ‘i mL
final extract results in only a negligible 1%change in the final extract volume).
Option 2 -Adjust spike solution to a known volume with sample.in this case the sample
concentration must be adjusted.When tho vclums of spike solution cxcacds 1%of tha total MS
volume the sample concentration must be adjusted prior to determining spike recovery.
The general equation for spike recovery is as follows:
%R =amt.of target in spiked sample —amt.of target in unspiked sample
,W(C,()l‘l§J_-..QLlTiElS,S)..__.__l.QQtlG.or mass)_______\x 100
amt.of tangot spikcd Into this sample
(conc.or mass)
To apply this to the sample preparation schemes described above,refer to the following examples.
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#20 PAR Laboratories,lnc.
M:-ltrix Spiking Policy and Technical Assistance
Page Z ol'3
Spike Preparation Examples
Option 1 -it the spike solution volume is equal to 1%or less of the total sample volume,direct
subtraction oi the unsplked sample is allowed.
Option 1 Example:
0.5 mls of a 1000 mg/L standard spike added to 100 mls of sample has a theoretical value of 5
mglL.,
(A)The spiked sample recovery is 5.1 mg/L
(B)if the unspiked sample result is 0.5 mg/L
(C)Theoretical value is 5.0 mg/L
The Percent Recovery =spiked sample recovery (A)—unspiked sample result (B)divided by
theoretical value (C)X 100 or
5.1 —0.5 X 100 =92%recovery A—B X 100 =Percent recovery
5 0 C
Option 2 -Adjust spike solution lo a known volume with sample.in this case the sample concentration
must be adjusted.
Option 2 Example 1:
10 mls of spike (concentration 60 mg/L)brought to 100 mls with sample the theoretical MS value is
5 mgiL.
(A)The spiked sample recovery is 5.1
(B)If the unspiked sample result is 0.5 mgiL
(C)%sample is 0.90 (sample volume used (90)divided by final volume (100))
(D)Theoretical value is 5.0 mg/L
The Percent Recovery =spiked sample recovery (A)Q (unsplked sample result (B)x %sample
(C))divided by theoretical value (D)X 100 or
5.1 -__(Q.5yx 0.9)X 100 =93%recovery 51-(fB__;-t C)X 100 =Percent recovery
5.0 D
Option 2 Example 2:Larger spike volume
25 mls of spike (concentration 50 mg/L)brought to 250 mls with sample the theoretical MS value
is 5 mg/L.
(A)The spiked sample recovery is 5.6
(B)If the unspiked sample result is 0.5 mg/L
((3)%sample is 0.90 (sample volume used (225)divided by final volume (250))
(D)Theoretical value is 5.0 mg/L
The Percent Recovery =spiked sample recovery (A)-(unsplked sample result (B)x %sample
(C))divided by theoretical value (D)X 100 or
5.6 -(0.5 x 0.9iX 100 =103%recovery A—(B x C1X 100 =Percent recovery
5.0 D
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#20 PAR Laboratories,lnc.
Matrix Spikihg Policy and Tcclmical Assistance
Page 3 oi'3
Corrective Actionlqualifications for MS
Spike accuracy is usully based on a range of percent recovery (e.g.,BO»12D%).Refer to the method of
choice for specific acceptance criteria for the matrix spikes until the laboratory develops or adopts
statistically valid.laboratory-specific performance criteria for accuracy.If a MS fails,and the LCS is
acceptable,quality the data for the MS sample.Repeated failures for a specific matrix may require use of
an alternate method or method of standard addition.Base the sample batch acceptance on the results of
the LCS analyses (and other quality control results)rather than the MS alone,because the matrix of the
spiked sample may interfere with the method performance.If a MS and the associated LCS fail,re-
prepara and reanalyze aifected samples.
Post Digestion Spikes (PDS1
Post Digestion Spikes (PDS)are used for some analyses (e.g.,metals)to assess the ability of a method
to successfully recover target analytes from an actual sample matrix after the digestion process has been
performed.The PDS results are used with MS results to evaluate matrix interferences.The MS and PDS
should be prepared from the same environmental sample.A PDS is not to be analyzed in place of a MS.
Post Digestion Spikes must be reported as post-digested and must not be misrepresented as pre-
digested spikes.(Exception:TCLP and SPLP samples are always spiked post digestion.)
Corrective Actionlflualifications for Post Digestion Spikes
In general.If the MS recovery for an analyte does not fall within the quality control acceptance range but
the PDS recovery is acceptable,then a matrix affect (associated with the prparetory process)should be
suspected and the unspiked sample results must be qualified on the basis of the matrix spike recovery.
However,when historical data for the effect does not exist,the laboratory would normally be expected to
perform a second digestion and reanalysis of the MS to confirm the result.The result would be confirmed
if the MS recoveries and PDS recoveries for both sets of analyses were similar in magnitude and bias.
When both the MS recovery and PD5 recovery for a particular analyte falls outside of quality control
acceptance range in the same manner (i.e..the PDS and MS failures are of similar magnitude and the
direction of bias is the same),confirmatory analyses are unnecessary but the data must be qualified.
Parameters Excluded from MS Requirements
Acidity Alkalinity
BODICBOD Aquatic Humic Substances
Chlorophyll All Bacteriological Parameters
Color —ADM!Color —PtCo
Conductivity Dissolved Oxygen
lgnitablllty 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.)
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NCDENRNorthCarolinaDepartmentofEnvironment and Natural Resources
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Pat l\/lctlrory Donald R.van der \/aart
Governor Secretary
I June 17,2015
‘Z0
lMr.Russell Everett
lPAR Laboratories,lnc.
lBox 411483
;Charlotte,NC 28273
._._.0)__.__,_L___
ubject:North Carolina Wastewater/Groundwater Laboratory Certification (NC \/\IW/GW LC)
Maintenance Inspection
l
iDear Mr.Everett:
§Enclosed is a report for the inspection performed on April 21,2015 by staff of the NC WW/GW LC
program and EPA Region 4.I apologize for the delay in getting this report to you.Where finding(s)
are cited in this report,a response is required.Within thirty days of receipt,please supply this office
with a written item for item description of how these finding(s)were corrected and include an
limplementation date for each corrective action.If the finding(s)cited in the enclosed report are not
corrected,enforcement actions may be recommended.For certification maintenance,your
llaboratory 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.lf you wish to obtain an electronic copy of this
report by email or if you have questions or need additional information,please contact us at (828)
296-4677.
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Sincerely,
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A 6)“?7”““*1
Gary Francies,Technical Assistance/Compliance Specialist
,Division of Water Resources
§Attachment
‘cc:Beth Swanson
Ray Terhune
i Wes Bell
l
Water Sciences Section
NC Wastewater/Groundwater Laboratory Certification Branch
,1623 Mall Service Center.Raleigh.North Carolina 27699-1623
l Location:4405 Reedy Creek Road,Raleigh,North Carolina 27607
1 Phone:919~733v3908 i FAX:[phone]
lnternet:[e-mail]
An Equal Opportunity '2 Affirrnailve Action Employer
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