TRCTRC Environmental Corporation
Boott Mills South,
Lowell, MA 0185.•s- (508) 970-5600
SDMS DocID 3915
April 17, 1995
Ms. Christine ClarkRegional Sample Control CoordinatorU.S. Environmental Protection AgencyEnvironmental Services Division60 Westview StreetLexington, MA 02173-3185
V 7 1
Reference:
Subject:
Contract No. 68-W9-0033, ARCSWork Assignment No. 22-1LB7Gallups Quarry Superfund Site CT WASTE I ... ,..,,
CT SuPiiRKii li-i
Deliverable: Data Validation ReportCase #23127 SDG: MACZ49CLP Lab: Skinner & ShermanMetals: 5/aqueous/MACZ49, MACZ50, MAEP14 - MAEP16Cyanide: 5/aqueous/MACZ49, MACZ50, MAEP14 - MAEP16
Dear Ms. Clark:
In accordance with the reporting requirements of the subject work assignment, enclosed is aData Validation Report for case 23127 which was generated by Quality Specialists &Environmental Analysts, Inc., TRCC's Data Validation Subcontractor for this workassignment. The Tier HI validation was performed on analytical data of samples collected byTRCC at the Gallups Quarry Superfund Site during the sampling event conducted on January11, 1995.
If you have any questions, please feel free to contact me at (508) 656-3553.
Sincerely yours,
Edward, MacKinnonLead Chemist
Enclosures
cc: Leslie McVickar/EPA RPMCathy Lielausis/TRCC Project ManagerPaul HughesATRCC Program Manager (letter only)
Offices in California, Colorado, Connecticut, Illinois, Louisiana, Massachusetts, Minnesota, Nevada, New Jersey, New Mexico,
New York, North Carolina, Ohio, Oregon, Texas, Utah and Wyoming A TRC Company
Printed on Recycled fsper An Equal Opportunity Employer
ORGANICS COMPLETE SDG FILE (CSF) INVENTORY SHEET
LABORATORY NAME CEIMIC CORPORATIONCITY/STATE NARRAGANSETT, RICASE NO. ^ /^~7 SDG NO. A T f f K ? SDG NOS. TO FOLLOW
SAS NO.CONTRACT NO. btfly^Aj /sow NO. fiLium r?
v
All documents delivered in the complete SDG file must be original documentswhere possible. (REFERENCE EXHIBIT B, SECTION II and SECTION III.)
PAGE NOs. CHECKFROM TO LAB EPA
0. Sample Data Summary Package(Sent to SMO Only)1. Inventory sheet (Form DC-2) (Do not number)2. Cover Sheet3 . SDG Case Narrative4. SDG Cover Sheet/Traffic Report5. Volatiles Data
a. QC SummarySystem Monitoring Compound Summary(Form II VOA)
Matrix Spike/Matrix Spike DuplicateSummary (Form III VOA)
Method Blank Summary (Form IV VOA)GC/MS Instrument Performance Check(Form V VOA)
Internal Standard Area and RT Summary(Form VIII VOA)
b. Sample DataTCL Result - (Form I VOA)Tentatively Identified Compounds(Form I VOA-TIC)
Reconstructed total ion chromatograms(RIC) for each sample
For each sample:Raw spectra and background-subtractedmass spectra of target compoundsidentified
Quantitation reportsMass spectra of all reported TICs withthree best library matches
c. Standards Data (All Instruments) f—L 4±L?Initial Calibration Data (Form VI VOA)RICs and Quan Reports for all StandardsContinuing Calibration Data (Form VII VOA)RICs and Quantitation Reports for allStandards
d. Raw QC DataBFBBlank DataMatrix Spike/Matrix Spike Duplicate Data
FORM DC-2-1 Page 1 of 4
ORGANICS COMPLETE SDG FILE (CSF) INVENTORY SHEET (Cont.)
CASE NO. r^ S \<±~1 SDGSAS
NO.NO.
/VTH 1$ SDG'
NOS. TO FOLLOW
PAGE NOs. CHECKFROM TO LAB EPA
6. Semivolatiles Dataa. QC Summary
Surrogate Percent Recovery Summary(Form II SV)
MS/MSD Summary (Form III SV)Method Blank Summary (Form IV SV)GC/MS Instrument Performance Check(Form V SV)
Internal Standard Area and RT Summary(Form VIII SV)
b. Sample Data 0' /? 7~ TCL Results (Form I SV-1, SV-2)Tentatively Identified Compounds (Form ISV-TIC)
Reconstructed total ion chromatograms(RIC) for each sample
For each sample:Raw spectra and background-subtractedmass spectra of target compounds
Quantitation reportsMass spectra of TICs with three best
library matchesGPC chromatograms (if GPC performed)
Standards Data (All Instruments)Initial Calibration Data (Form VI SV-1,
SV-2)RICs and Quan Reports for all StandardsContinuing Calibration Data (Form VIISV-1, SV-2)RICs and Quantitation Reports for allStandards
Semivolatile GPC Calibration Data-UVdetector traces
Raw QC Data ^"^ 'DFTPPBlank DataMatrix Spike/Matrix Spike Duplicate Data
7. Pesticides
QC SummarySurrogate Percent Recovery Summary(Form II PEST)
MS/MSD Duplicate Summary (Form III PEST)Method Blank Summary (Form IV PEST)
FORM DC-2-2 Page 2 of 4
ORGANICS COMPLETE SDG FILE (CSF) INVENTORY SHEET (Cont.)
CASE NO. «23>(V7 SDG NOSAS
• f \ J j t
NO.L{tf SDG NOS. TO FOLLOW
PAGE NOs.FROM TO
7. Pesticides (cont.)b. Sample Data
TCL Results
CHECKLAB EPA
d.
Organic Analysis DataSheet (Form I PEST)
Chromatograms (Primary Column)Chromatograms from second GC columnconfirmation
GC Integration report or data systemprintout
Manual work sheetsFor pesticides/Aroclors confirmed byGC/MS, copies of raw spectra andcopies of background-subtracted massspectra of target compounds (samples& standards)
Standards DataInitial Calibration of Single ComponentAnalytes (Form VI PEST-1 and PEST-2)
Initial Calibration of MulticomponentAnalytes (Form VI PEST-3)
Analyte Resolution Summary (Form VIPEST-4)
Calibration Verification Summary (FormVII PEST-1)
Calibration Verification Summary (FormVII PEST-2)
Analytical Sequence (Form VIII PEST)Florisil Cartridge Check (Form IXPEST-1)
Pesticide GPC Calibration (Form IXPEST-2)
Pesticide Identification Summary forSingle Component Analytes (Form XPEST-1)
Pesticide Identification Summary forMulticomponent Analytes (Form XPEST-2)
Chromatograms and data system printoutsA printout of retention times andcorresponding peak areas or peak heightsPesticide GPC calibration data - UVdetector traces
Raw QC DataBlank DataMatrix Spike/Matrix Spike Duplicate Data
676
FORM DC-2-3 Page 3 of 4
ORGANICS COMPLETE SDG FILE (CSF) INVENTORY SHEET (Cont.)
CASE NO. SDG NO.SAS NO.
SDG NOS. TO FOLLOW
10,
11
12.
PAGE NOs.FROM TO
8. Miscellaneous Data
Original preparation and analysis forms orcopies of preparation and analysis logbookpages
Internal sample and sample extract transferchain-of-custody records
Screening recordsAll instrument output, including strip chartsfrom screening activities (describe or list)
EPA Shipping/Receiving Documents
Airbills (No. of shipments ^3 )Chain-of-Custody RecordsSample TagsSample Log-In Sheet (Lab & DC1)Miscellaneous Shipping/Receiving Records
(describe o£ list)__>7pv\,
"733
?J*iQ^Dl K / y cs-* [\in,^
<3 0Internal Lab Sample Transfer Records and
Tracking Sheets_(describe or list)Lrz-JJ flj^x /I I 7~6L>T\ J^I rt T ^<5^
<7Other Records (describe or list)
telephone Communication Log ^-y^
"GU
ZS- ^22^<£&SZO<g-2^
CHECKLAB EPA
Completed by:(CLP Lab)
Audited by:(EPA) \ature) (Printed Name/Title) ' (Date)
FORM DC-2-4 Page 4 of 4
IUALITY SPECIALISTS & ENVIRONMENTAL ANALYSTS, INC.
Environmental Data Validation & Interpretation
April 11,1995
Ms. Christine ClarkRegional Sample Control CoordinatorU.S. Environmental Protection AgencyEnvironmental Services Division60 Westview StreetLexington, MA 02173-3185
Dear Ms. Clark:
RE: Prime Contract/Subcontract: 68-W9-QQ33/1-636-999-OSEAWork Assignment #: 0163602301LB73Case #: 23127 , SDG #: MACZ49Lab Name:Site Name:Metals:Cyanides:
Skinner & ShermanGalluos Ouarrv Suoerfund Site
55
A Tier III validation was performed on the inorganic analytical data from Case 23127, five aqueous samplescollected by TRC Environmental Corporation at the Gallups Quarry Superfund site. The data was evaluatedbased on the following parameters:
* data completeness* holding times* calibration
laboratory and field blank analysesmatrix spike recoverieslaboratory and field duplicates
* laboratory control sample results* furnace atomic absorption results* serial dilution results* detection limit results* sample results
* All criteria were met for this parameter
P.O. Box 670
QSEADunbar, West Virginia 25064 Phone/Fax:l
304-776-0400/0403
Table 1 summarizes the validation recommendations which were based on the following information:
- Laboratory and Field Blank Analyses:
Blank detections are summarized below:
Maximum Concentration Action LevelElements (ug/L) (ug/L)Barium
CadmiumCalciumCopper
IronLead
ManganeseNickel
Potassium
SodiumZinc
1.51.8
246.78.214.02.1
1.6
3.1
(82.3)
153.014.8
7.5
9.01 ,233.5
41.070.010.58.0
15.5(411.5)
765.074.0
Value > IDL and < Action Level = Report value uValue > IDL and > Action Level = Report value unqualified
Batch results have been modified in accordance with the criteria above.
- Laboratory and Field Duplicates:
Iron results were greater than 5x CRDL for both MAEP16 and MAEP16D, and precision was outsidethe +/- CRDL range. Positive results for this batch (samples MACZ50, MAEP14 and MAEP16) areflagged T.
- Matrix Spike Recoveries:
Matrix Spike %R result was outside the criteria for cyanide. All samples were flagged as estimated.
Very truly yours,QSEA, Inc.
Steven J. LaskyInorganic Data Reviewer
SJL/irs
cc: EPA - Leslie McVickar
MA49R.WPS Page 2 of 3 - TRC SDG #MACZ49 Validation Report
Gallups Quarry Superfund SiteCase #MACZ49
Table I. Recommendation Summary
ElementAluminumAntimonyArsenicBarium
BerylliumCadmiumCalcium
ChromiumCobaltCopper
IronLead
FlagAAAA1
AA'A1
A
AA'
A>, J2
A1
ElementMagnesiumManganese
MercuryNickel
PotassiumSelenium
SilverSodium
ThalliumVanadium
ZincCyanide
FlagAAiAA'
A1
AA
AAAAi
J'
DATA SUMMARY 1CEY
A - Accept all data.
A1 - Accept data, raise the sample detection limit(s) as needed due to blank contamination., or report results asunqualified
J1 - Estimate all positive values (J) and detection limits (UJ) due to low matrix spike recoveries. Theseestimated results would be minimum values.
J2 - Estimate all positive values (J) due to poor precision between laboratory duplicates..
MA49R.WPS Page 3 of 3 - TRC SDG 8MACZ49 Validation Report
TABLE MACZ49-AINORGANIC DATA SUMMARY TABLE
VALIDATED DATA FORTRC ENVIRONMENTAL CORPORATIONCALLUPS QUARRY SUPERFUND SITE
CASE #23127 SDO #MACZ49LABORATORY: SKINNER AND SHERMAN LABS, INC.
SAMPLEDSAMPLE LOCATIONLAB SAMPLE IDSAMPLE DATESAMPLE MATRIXDILUTION FACTOR% SOLIDS
CASi7429-90-57440-36-07440-38-27440-39-07440-41-77440-43-97440-70-27440-47-37440-4847440-50-87439-89-67439-92-17439-95-47439-96-57439-97-*7440-02-07440-09-77782-49-27440-22-47440-23-57440-28-07440-62-27440-66-65955-704)
ANALYTEAluminum
AntimonyArsenicBarium
Beryllium
CadmiumCalcium
ChromiumCobaltCopper
IronLead
MagnesiumManganese
MercuryNickel
PotassiumSelenium
SilverSodiumThalliumVanadium
ZincCyanide
METHODFflP/CVTC
PcvPPPPPPPPc
IDLUG/L22.517.82.01.20.31.4
35.82.12.32.75.60.923.00.70.22.8
78.73.04.137.91.82.43.610.0
MACZ49TARBOX-4001061-01S01/11/95WATER
1.0N/A
CONCUG/L26.617.8 ~l2.080.10.301.4
175002.12.3
32.96.91.9
251023.40.202.8
26503.04.1
353001.82.414.210.0
Q
UU
UU
UUUUU
UU
UU
UUUUJ
MACZCOUlfefMg*4301M1-02S01/11/95WATER
UON/A
CONCUG/L22.517.82.05.4
0.301.4
332002.1246.1
68.41.9
26700.700.20
2.827203.04.1
106001.82.47.710.0
QUUUUUU
UUU
U
UUU
UU
U
UUUJ
MAEP14MW-107T§106143801/1 1/MWATER
1JO
N/ACONCUG/L19017.82.05.6
0.301.4
99103.9
2.35.52181.1
139036.40.202.9
22303.04.1
69101.83.93.610.0
Q
UUUUU
UU
U
UU
UU
U
UUJ
MAEP16EB-1
01061-03S01/1 MSWATER
1J»N/A
CONCUG/L22.517.82.01.2
040141812.12.33.114.02.1
23.00.950.2024
78.73.04.1153142.47.410.0
QUUUUUUU
UUUUUUUUU
UUU
UUUUJ
CROLUG/L2006010
20055
60001060251003
5000160.240
5000510
500010502010
Analytical Method:F = FurnaceP B (CP/Flame AACV - Cold VaporC = Cokmmetric
QSEA File: MA49M Page! of2
TABLE MACZ49-AINOROAMC DATA SUMMARY TABLE
VALIDATED DATA FORTRC ENVIRONMENTAL CORPORATIONGALLUPS QUARRY SUPERFUND SITE
CASE *23127 SDG IMACZ49LABORATORY: SKINNER AND SHERMAN LABS, INC.
SAMPLE IDSAMPLE LOCATIONLAB SAMPLE IDSAMPLE DATESAMPLE MATRIXDILUTION FACTOR% SOLIDS
CAS*7429-80-57440-36-07440-38-27440-39-3744041-77440-43-97440-70-27440-47-37440-48-47440-50-87439-89-67439-92-17439-95-47439-96-57439-97-67440-02-07440-09-77782-49-27440-22-47440-23-57440-28-07440-62-27440-66-65955-70-0
COMPOUNDAluminumAntimonyArsenicBarium
BerylliumCadmiumCalcium
ChromiumCobaRCopper
IronLead
MagnesiumManganese
MercuryNickel
PotassiumSelenium
SilverSodiumThalliumVanadium
ZincCyanide
METHODrmcvtc
cv
ppppppc
IDL(U»M
22.517.82.01.20.31.4
35.82.12.32.76.60.923.00.70.22.8
78.73.04.137.91.82.43.610.0
MAEP16MW-10580108143891/11/95WATER
1jON/A
CONCUG/L47.817.82.04.00.31.4
269002.12.32.7
11601.5
238011.90.22.8
15903.04.1
44101.82.74.210.0
Q
UUUUU
UUU
U
UU
UU
U
U
UJ
CRDL(MM.)
200601020056
50001060251003
6000150.240
6000510
600010602010
Analytical Method:F* FurnaceP«rCP/FlameAACV * CoM VaporC a Colorimetric
QSEA File: MA49M Page 2 of 2
JjF
CASE NO.LABORATORY
SDG#SOW#DPO: ACTION
INORGANIC REGIONAL DATA ASSESSMENTRegion
23127Skinner and Sherman
MACZ49ILM03.0
FYI
SITENO. OF SAMPLES/MATRIXREVIEWERREVIEWER'S NAMECOMPLETION DATE
Gallups Quarry Superfund
6 waterQSEAJnc.
Steven J. Lasky04/03/96
OATA ASSESSMENT SUMMARY
: ;' . - ' - — • « *
1. HOLDING TIMES
2. CALIBRATIONS
3. BLANKS
4.ICS
6. LCS
6. DUPLICATE ANALYSIS
7. MATRIX SPIKE
8. MSA
9. SERIAL DILUTION
10. SAMPLE VERIFICATION
11. OTHER QC
12. OVERALL ASSESSMENT
0
O
X
O
0
0
O
N/A
O
O
0
O
AA HB CYAIflOE
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
N/A
O
0
O
N/A
O
O
O
N/A
O
O
O
O
0
O
O
N/A
O
O
M
N/A
O
O
O
0
O = Data had no problems/or qualified due to minor problems.M = Data qualified due to major problems.Z * Data unacceptable.X= Problems, but do not affect data.
ACTION ITEMS
AREAS OF CONCERN: x-DETECTioN LIMITS WERE RAISED DUE TO BLANK CONTAMINATION.M»%R WAS OUTSIDE CRITERIA FOR CYANIDE: ALL DATA ESTIMATED.LAB DUPLICATE RESULTS FOR IRON CAUSED ESTIMATION OF POSITIVE RESULTS FOR MACZ60, MAEP14.MAEP16
NOTABLE PERFORMANCE:
FormlNT3-1t
QSEA File: MA49F326.WB2 - 26
Inc.*•REGION I Site Name Gallups Quarry SuperfundData Review Worksheets
REGION I REVIEW OF INORGANICCONTRACT LABORATORY DATA PACKAGE
TIER III VALIDATION LEVEL
The hardcopied skinner and Sherman Labs data package received at QSEA, Inc. has been reviewed and the qualityassurance and performance data summarized. The data review included:
Case No. _ 23127 _ SAS No. _ N/A _ Sampling Date(s) _ 01/11/95 _SDG. No. _ MACZ49 _ Matrix Water _ Shipping Date(s) _ 01/12/95 _No. of Samples 5 Metals. 6 cyanide Date Rec'd by Lab _ 01/13/95 _
Traffic Report Nos.: -999909 nMCz^/? fllACz.'fr mAEfi'-l -r>M b
Trip Blank No.: NoneEquipment Blank No. MAEPISField Duplicate Nos.: NONE
SOW # ILM03.0 requires that specific analytical work be done and that associated reportsbe provided by the laboratory to the Regions, EMSL-LV, and SMO. The general criteria used to determine theperformance were based on an examination of:
» Data Completeness * Field Duplicates• Holding Times • Lab Control Sample Results* Calibrations * ICP Serial Dilution Results* Blanks * Detection Limit Results• ICP Interference Check Results « Sample Quantitation* Matrix Spike Recoveries• Laboratory Duplicates
Overall Comments DATA WAS ESTIMATED DUE TO POOR MATRIX SPIKE RECOVERY FOR CYANIDE AND LACK OF PRECISION FORIRON LAB DUPLICATES. BLANK CONTAMINATION WAS FOUND FOR 10 ANALYTES, CAUSING MODIFICATION OF RESULTS.
Definitions and Qualifiers:
A - Acceptable Data.J - Approximate data due to quality control criteria.R - Reject data due to quality control criteria.U - Analyte not detected
Reviewer Steven J. Lasky Date: 04/03/96
Form INT3-1
QSEA File: MA49F326.WB2 - 1
Q,siREC
'Dab
\.
7 A J*f /~i/l; JA/C.~'~~~< ~~~<^~ ~~~~^^^,^,^~^^,^^,~^^^, / ^^<^,^,,
jlONI3 Review Worksheets
DATA COMPLETENESS
MISSING INFORMATION DATE LAB CONTACTED DATA RECEIVED
None
FormlNn-3
******
QSEA File: MA49F326.WB2 - 2
QsiREC
. DaU
II.
?A Jmr ~~~ ~~ ~ ~~u<£ JL* Jl w v\*' »
SIONI3 Review Worksheets
HOLDING TIMES
Complete table for all samples and enter an 'X' beside the analysis date for samples not within criteria
hg CYANIDE OTHERSSAMPLE » DATE DATE DATE DATE pH ACTION
SAMPLED ANALYSIS ANALYSIS ANALYSIS
MACZ49
MACZ50
MAEP14
MAEP15
MAEP16
MAEP16D
MAEP16S
01/11/95
01/11/95
01/11/95
01/11/95
01/11/95
01/11/95
01/11/95
01/23/95
01/23/95
01/23/95
01/23/95
01/23/95
01/23/95
01/23/95
01/18/95
01/18/95
01/18/95
01/18/95
01/18/95
01/18/95
01/18/95
01/31/95
01/31/95
01/31/95
01/31/95
01/31/95
01/31/95
01/31/95
CN=12Met=1.5CN=12Met=2.0CN=12MeMOCN»12Met=2.0CN=12Met=2.0CN=12Mct=2.0CN*12Met=2.0
ACCEPT
ACCEPT
ACCEPT
ACCEPT
ACCEPT
ACCEPT
ACCEPT
METALS - 180 DAYS FROM SAMPLE COLLECTIONMERCURY • 28 DAYS FROM SAMPLE COLLECTIONCYANIDE - 14 DAYS FROM SAMPLE COLLECTION
ACTION.1 . If holding times are exceeded all positive results are estimated (J) and non-detects
are estimated (UJ).
2. If holding times are grossly exceeded, the reviewer may determine that non-detectsare unusable (R).
FermMTS-3
QSEA Rto: MA49F326.WB2 - 3
QSEA,1
REGION 1' Data Revie
III. A. IN!
1.
ACTIO
If any <
For
For
r'yifA/C. '"""' ~~ *-^ «•« ™ •"-' ru
w Worksheets
5TRUMENT CALIBRATION (Section 1)
Recovery Criteria
List the analytes which did not meet the percent recovery (%R) criteria for Initial or ContinuingCalibration.
DATE ICWCCV* ANALYTE %R ACTXm SAMPLES AFFECTED
NONE
NS:
»nalyte does not meet the %R criteria follow the actions stated below:
Positive Results:
Accept Estimate ) fUject(R)
Metals 90-110%R 75-89%R, 111-125%R <75%R, >125%RMercury 80-1 20%R 65-79%R, 121-135%R <65%R, >135%RCyanide 85-115%R 70-84%R, 116-130%R <70%R, >130%R
Non-detected Results:
Accept Estimate (UJ) RajectCR)
Metals 90-125%R 75-89%R <75%R, >125%RMercury 80-1 35%R 65-79%R <65%R, >135%RCyanide 85-1 30%R 70-84%R <70%R, >130%R
FonnMn-4
GSEA FH«: MA49F326.WB2 - 4
CCA Jvi/~ ~ ~ ~ ~OJJtti., .I/t-C'. ~~~.— ~~~^^,^,,
REGION IData Review Worksheets
III. B. INSTRUMENT CALIBRATION (Section 2)
2. Analytical Sequence Mark One
a. Did the laboratory use the proper number of standardsfor calibration as described in the SOW? Yes X No
b. Were calibrations performed at the beginning of eachanalysis? Yes X No
c. Were calibration standards analyzed at the beginningof sample analysis and at a minimum frequency of tenpercent or every two hours during analysis, whicheveris more frequent? Yes X No
d. Were the correlation coefficients for the calibrationcurves for AA, Hg, and CN >/= 0.995? Yes X No
e. Was the standard at 2xCRDL analyzed for all ICPanalyses? Yes X No
If NO,
The data may be affected. Use professional judgement to determine the severity of the effect andqualify the data accordingly. Discuss any actions below and list the samples affected.
FocmMTS-C
QSEA File: MA49F326.WB2 - 5
INORGANIC INITIAL CALIBRATION VERIFICATION
File Name ICV Date of Initial Calibration 01/27/95
ICP Analyte ALUMINUM
1949.2 \ 1878.0 100
Lab Value 103.8
103.8 %R
File Name N/A Date of Initial Calibration
Furnace Analyte Lab Value
File Name
Analyte
%R
ICV Date of Initial Calibration 01/23/95
Mercury Lab Value 100.4
5.0 \ 5.0 100 100.4 %R
File Name
Analyte
%R
ICV Date of Initial Calibration 01/18/95
Cyanide Lab Value 106.7
100.3 / 94.0 100 106.7 %R
FormtNTO-M
QSEA File: MA49F326.WB2 - 6
SEA, Inc.
INORGANIC CONTINUING CALIBRATION VERIFICATION
File Name CCV2 Date of Continuing Calibration 01/27/95
ICP Analyte BARIUM
2455.6 \ 2500.0
Lab Value 98.2
100 98.2 %R
File Name
Furnace Analyte
Date of Continuing Calibration
N/A Lab Value
File Name
Analyte
%R
CCV1 Date of Continuing Calibration 01/23/95
Mercury Lab Value 100.5
2.01 \ 2.0 100 100.5 %R
File Name
Analyte
%R
CCV3 Date of Continuing Calibration 01/18/95
Cyanide Lab Value 98.4
196.9 \ 200.0 100 98.5 %R
Form INT3-5B
QSEA File: MA49F326.WB2 - 7
Q SEA, Im
REGION 1• Data Review V\
IV. A. BLANh
List thewater t
1. Lat
2. Eq
3. Fre
a.
b.
If NO,Th€
and qu
• •
Worksheets
(ANALYSIS RESULTS (Sections 1-3)
5 blank contamination in Sections 1 & 2 below. A separate worksheet should be used for soil and)lanks.
moratory Blanks
DATE
01/27/95
01/27/95
01/27/95
01/27/95
01/27/95
ICB/CCB*
ICB1/CCB2
ICB1
ICB1/CCB1/CCB3
ICB1/CCB1
ICB1/CCB1/CCB3
PREP BLANK ANALYTE CONC^ug/U
Barium
Cadmium
Calcium
PBW Copper
PBW Iron
1.5/1.4
1.8
246.7/113.9/73.8
8.2/7.0/6.65
7.9/12.9/5.9/10.57
jipment/Trip Blanks
DATE
01/27/95
01/27/95
01/27/95
01/31/95
01/27/95
EQUIP BLANK *
MAEP15
MAEP15
MAEP15
MAEP15
MAEP15
quency Requirements
Was a preparation blank analyzed for eacfor every 20 samples and for each digestk
Was a calibration blank run every 10 samevery 2 hours whichever is more frequent'
j data may be affected. Use professional jalify the data accordingly. Discuss any ad
ANALYTE CONC.(u0/L)
Calcium 181
Copper 3.1
Iron 14
Lead 2.1
Manganese 0.95
h matrix,an batch? Yes X No
pies or? Yes X No
udgement to determine the severity of the effectlions below, and list the samples affected.
FormMn4
QSEA File: MA49F326.WB2 - 6
Q SEA, Im
REGION 1' Data Review V\
IV. A. BLANK
List thewater t
1. Lat
2. Eqi
^ .
Worksheets
C ANALYSIS RESULTS (Sections 1-3)
! blank contamination in Sections 1 & 2 below. A>lanks,
moratory Blanks
DATE
01/27/95
01/27/95
01/27/95
01/27/95
separate worksheet should be used for soil and
ICB/CCB* PREP BLANK ANALVTE CONC4V/U
ICB1/CCB1
ICB1
CCB2
ICB1/CCB1/CCB2/CCB3 PE
Manganese
Nickel
Potassium
IW Zinc
1.6/0.8
3.1
-82.3
14.8/5.9/4.9/3.7/4.94
jipment/Trip Blanks
DATE
01/27/95
01/27/95
EQUIP BLANK * ANALYTE CONC.(ug/L)
MAEP15 Sod
MAEP15 Zi
ium 153
nc 7.4
3. Frequency Requirements
a. Was a preparation blank analyzed for each matrix,for every 20 samples and for each digestion batch? Yes X
b. Was a calibration blank run every 10 samples orevery 2 hours whichever is more frequent?
No
Yes X No
If NO.The data may be affected. Use professional judgement to determine the severity of the effect
and qualify the data accordingly. Discuss any actions below, and list the samples affected.
FormMT34
QSEA Fit* MA49F326.WB2 - 9
SEA,REGION IData Review Worksheets
IV. B. BLANK ANALYSIS RESULTS (Section 4)
4. Blank Actions
The Action Levels for any analyte is equal to five times the highest concentration of that element'scontamination in any blank. The action level for samples which have been concentrated or dilutedshould multiplied by the concentration/dilution factor. No positive sample result should be reportedunless the concentration of the analyte in the sample exceeds the Action Level (AL). Specific actionsare as follows:
a. When the concentration is greater than the IDL, but less than the Action Level, report the sampleconcentration detected with a U.
b. When the sample concentration is greater than the Action Level, report the sample concentrationunqualified.
MATRIX: Water
ELEMENT MWC. CONG/ AU(US/U <U9/U
Barium
Cadmium
Calcium
Copper
Iron
Lead
Manganese
1.5
1.8
246.7
8.2
14
2.1
1.6
7.5
9
1233.5
41
70
10.5
8
MATRIX: Water
EUEMENT : - :: WAX.:CONCjr :: '. ' ••'.'*&. ::::: '"<ufl/U tugm
Nickel
Potassium
Zinc
Sodium
3.1
-82.3
14.8
153
15.5
-411.5
74
765
NOTE: Blanks analyzed during a soil case must be converted to mg/kg in order to compare them withthe sample results.
Cone, in ug/L X (Volume diluted to (200ml)/Weight digested (1gram)) X (1L/1000ml) X (1000gm/1kg)X(1mg/1000ug) = mg/kg
Multiplying this result by 5 to arrive at the action level gives a final result in mg/kg which can then becompared to sample results.
Form INT3-7
QSEA File: MA49F326.WB2 - 10
QSEA,1
REGION 1Data Revie
V. A. ICF
1.
Lis
AC
If a
.
TIC.
w Worksheets
> INTERFERENCE CHECK SAMPLE (Sections 1 & 2)
Recovery Criteria
t any elements in the ICS AB solution which did not meet the criteria for %R.
DATE ELEMENT
None
%R ACTION SAMPLES AFFECTED
flONS:
n element does not meet the %R criteria, follow the actions stated below:
PERCENT RECOVERY<50% 50-79% >120%
Positive Sample ResultsNon-detected Sample Results
2
R J JR UJ A
Frequency Requirements
Were Interference QC samples run at the beginning and endof each sample analysis run or a minimum of twice per 8-hourworking shift, whichever is more frequent? Yes X No
If NO,
The data may be affected. Use professional judgement to determine the severity of the effect andqualify the data accordingly. Discuss any actions below and list the samples affected.
FonnlNTS-8
QSEA Filo: MA49F326.WB2 - 11
SEA, Inc.REGION IData Review Worksheets
V. B. ICP INTERFERENCE CHECK SAMPLE (Section 3)
3. Report the concentration of any elements detected in the ICS A solution > 2xlDL that shouldnot be present.
Element
Sodium
CONO Detected m the ICS
927
Cone, of hitefNuwitftta<he ICS
AL CA FE MO
514927 529351 190348 543610
Estimate the concentration produced by the interfering element in all affected samples. See guidelinesfor examples. List the samples affected by interferences below:
SampleAffected
None
ElementAffected Sample Cone. (ug/L)
Sampte InterferantCone.
AL CA FE MO
EstimatedMM*.<ug/U
ACTIONS:
1. In general, the sample data can be accepted without qualification if the sample concentrations of Al, Ca,Fe, and Mg are less than 50% of their respective levels in the ICS solution.
2. Estimate (J) positive results for affected elements for samples with levels of interferents 50% or more of thatin the ICS solution.
3. Reject (R) positive results if the reported concentration is due entirely to the interfering element.
4. Estimate (UJ) non-detected results for which false negatives are suspect.
Give explanations for any actions taken below:
FonnlNT3-8
QSEA File: MA49F326.WB2 - 12
Q SEA, Inc.
ICP INTERFERENCE CHECK SAMPLE VERIFICATION
Lab File Name
Analyte
ICS%R
ICSAB-lnitial
ZINC Lab Value 102.4
1025.2 1001.0 x 100 102.4
Lab File Name
Analyte
ICS%R
ICSAB-Final
Magnesium Lab Value 103.3
551330.0 533685.0 x 100 103.3
Form INT3-9A
QSEA File: MA49F326.WB2 - 13
SEA, Inc.*REGION IData Review Worksheets
VI. MATRIX SPIKE
TR # MAEP16S * MATRIX: Water
1. Recovery Criteria
List the percent recoveries for analytes which did not meet the required criteria.
S - amount of spike addedSSR - spikes sample resultSR - sample result
Amrfytt SSR SR S %R Action
Cyanide 225.57 0 500 45.1 Apply "UJ"
Matrix Spike Actions apply to all samples of the same matrix.
ACTIONS:
1. If the sample concentration exceeds the spike concentration by a factor of 4 or more,no action is taken.
2. If any analyte does not meet the %R criteria, follow the actions stated below:
PERCENT RECOVERY00% 30%-74% >12fi%
Positive Sample ResultsNon-detected Results
JR
JUJ
JA
2 Frequency Criteria
a. Was a matrix spike prepared at the requiredfrequency? Yes
b. Was a post digestion spike analyzed for elementsthat did not meet required criteria for matrix spikerecovery? Yes
* A separate worksheet should be used for each matrix spike pair.
No
No
FannMT3-10
QSEA File: MA49F326.WB2 -14
SEA, Inc.
SAMPLE SPIKE ANALYSIS VERIFICATION
Sample ID
ICP Analyte
%R
MAEP16S
ANTIMONY Lab Value
504.390
100.9
0.000 \ 500.00 100 100.9 %R
Sample ID
Furnace Analyte N/A Lab Value
Sample ID
Analyte
%R
MAEP16S
Mercury Lab Value
0.768 0.000 1.00 100
76.8
76.8 %R
Sample ID
Analyte
MAEP16S
Cyanide Lab Value
%R 225.571 0.000 \ 500.00 100
45.1
45.1 %R
Fom INT3-10A
QSEA File: MA49F326.WB2 - 15
Q cJ7jd Tins* ~~~~~~~~~~^^~^~~~^~~~~~~~^'r*~r~~*~.r~~ '•''"".* " • " • ' . ' " - • •OjCulj JLlHs. . . • " . ' . • • TT .. . .-. •• ~~~
REGION 1Data Revie
VII. LABC
ListtcalcuIndie,elem
Labor
ACTI
1.
2.
sw Worksheets
)RATORY DUPLICATES
he concentrations of any analyte not meeting the criteria for duplicate precision. For soil duplicates,late the CRDL in mg/kg using the sample weight, volume, and percent solids data for the sample.3te what criteria was used to evaluate precision by marking an 'X' beside the RPD or CRDL for eachent.
MATRIX: Water
Element
AluminumAntimonyArsenicBariumBerylliumCadmiumCalciumChromiumCobaltCopperIronLeadMagnesiumManganeseMercuryNickelPotassiumSeleniumSilverSodiumThallium
VanadiumZincCyanide
CRDLWater ! Soil<uo/U <X) jmg/kg)2006010
200 j5
55000
10
5025100
55000
150.2
405000
510
50001050
2010
X
'.-.***&*#.-..MAEP16
1164.6
Popfcate*HMEPttD
1338.6
.. W0 . > •': ••-. . . ; , . . • ^
Actton
APPLY "J"
atory Duplicate Actions should be applied to all other samples of the same matrix type.
ONS:
Estimate (J) positive results for elements which have an RPD >20% for waters and > 35% for soils.
If sample results are less than 5x the CRDL, estimate (J) positive results for elements whose absolutedifference is >CRDL, (2xCRDL for soils). If both samples are non-detected, the RPD is not calculated(NC).
FonnlNT»-11
QSEA File: MA49F326.WB2 - 16
Q SEA, Inc.
DUPLICATE SAMPLE ANALYSIS
Sample ID
ICP Analyte
25927
MAEP16S
CALCIUM Lab Value 0.1
25899 / 25927 25899 / 2 100 = 0.11
Sample ID
Furnace Analyte
Sample -
File Name
N/A Lab Value
Duplicate / Sample Duplicate I 2 100 ERR
Sample ID
Analyte
NO DETECTIONS
MAEP16D
Mercury Lab Value N/A
Sample ID
Analyte
NO DETECTIONS
MAEP16D
Cyanide Lab Value N/A
PormMT3-11A
QSEA Hie: MA49F326.WB2 - 17
REGION IData Review Worksheets
VIM. FIELD DUPLICATES "NONE IDENTIFIED
List the concentrations of ail analytes in the field duplicate pair. For soil duplicates, calculate the CRDLin mg/kg using the sample weight, volume, and percent solids data for the sample. Indicate what criteriawas used to evaluate precision by marking an 'X' beside the RPD or CRDL for each element.
MATRIX: Water
Efcmer*
AluminumAntimonyArsenicBariumBeryllium JCadmiumCalciumChromiumCobaltCopperIronLeadMagnesiumManganeseMercuryNickelPotassiumSeleniumSilverSodiumThalliumVanadiumZincCyanide
Water(uo/U
2006010
20055
50001050251005
5000150.240
5000510
500010502010
CRDl
WSoil
frnsftS)"*«***••;-
None :' 'DupBcatft*
None "/•W* ;
W'Action •
Field Duplicate Actions should be applied to all other samples of the same matrix type.
ACTIONS:
1. Estimate (J) positive results for elements which have an RPD >30% for waters and > 50% for soils.
2. If sample results are less than 5x the CRDL, estimate (J) positive results for elements whose absolutedifference is >2xCRDL, (4xCRDL for soils). If both samples are non-detected, the RPD is not calculated(NC).
Form INTS-12
QSEA File: MA49F326.WB2 - 18
j^f S/*/4 lYLC" <^>^f^f^'^'^'*~'~~ff**f**r*'f^'*°*f*f**iff>f'r**'**'f~''**f**'f
REGION 1Data Revie
IX. LABOF
1. Aq
Lis
2. So
ListTh(
3. Fre
a.
•^f^r^r^t^ft^t^rrff^i+fir+rriivr^iritt+efi+ftr.i&.i*,
w Worksheets
?ATORY CONTROL SAMPLE
ueous LCS
t any LCS recoveries not within the 80-120% criteria and the samples affected.
DATE ELEMENT i : %R ACTION SAMPLES Af ECTED
None
id LCS
any analytes that were not within the control windows set by the EPA for the solid LCS sample.; 80-120% criteria is not used to evaluate solid LCS results.
ELEMENT LCS CONG, : CONTROL WINDOWS ACTION SAMPLES AFFECTED
ACTIONS:
PERCENT RECOVERYAqueous LCS <SO% 51-7*% >128%
Positive Sample Results R J JNon-detected Sample Results R UJ A
SottdLCS ^AfcsnfrolWtodOTW >t*»A Control WindowsPositive Sample Results J J
Non-detected Sample Results UJ A
quency Criteria
Was an LCS analyzed for every matrix, everydigestion batch, and every 20 samples?
Yes X No
FormlNTS-U
QSEA File: MA49F326.WB2 - 19
SEA, Inc.—
LABORATORY CONTROL SAMPLE VERIFICATION
Sample ID
ICP Analyte
Matrix
%R
LCS
BERYLLIUM Lab Value 94.5
WATER
451.7 478 100 94.50
Sample ID
ICP Analyte
Matrix
%R
LCS
POTASSIUM Lab Value 94.9
458.4 488 100 93.93 %R
Form INT3-13A
QSEA File: MA49F326.WB2 - 20
\ i-t J\ J* /YJ{* *-*+**** r*t +*+ **+ *w*w*f^-*^-r^-**^4'»^/^*>^J^w:*^^'^.r^'^/^<^>^''
REGION IData Review Worksheets
X. A. FURNACE ATOMIC ABSORPTION ANALYSIS
N/A _X
1. Duplicate Precision
_ Duplicate injections and one-point analytical spikes were performed"for all samples: duplicate injections agreed within +/- 20%.
_ Duplicate injections and/or spikes were not performed for the following samples/elements:
Duplicate injections did not agree within +/- 20% for samples/elements:
2. Post Digestion Spike Recoveries
Spike recoveries met the 85-115% recovery criteria for all samples.
Spike recoveries did not meet the 85-115% criteria but did not require MSA for thefollowing samples:
MSA was used to quantitate analytical results when contractually required.
Correlation coefficients >/= 0.995, accept results."Correlation coefficients < 0.995 for sample numbers/elements:
Method of Standard Addition (MSA) was not performed as required for samples/elements:
ACTIONS:1. Estimate (J) positive results if duplicate injections are outside +/- 20% RSD or CV.
2. If the sample absorbance is <50% of post digestion spike absorbance, the followingactions should be applied.
Positive Sample Results J OR R J JNon-detected Results R UJ A
3. Estimate (J) sample results if MSA was required and not performed.
4. Estimate (J) sample results if correlation coefficient was <0.995.
Form INT3-14
QSEA File: MA49F326.WB2 - 21
t f j_ii/i. IYIC ' ^^ **^i~^<~*'**r^***Hr~*< '4"^<™ '<t**'**'**rfir***^**N'-'*K'*^<n*' *' *' ^H^*i~^
REGION IData Review Worksheets
XI. INDUCTIVELY COUPLED PLASMA (ICP)
X Serial Dilutions were performedwithin ten percent of the originalbefore dilution.
Serial Dilutions were not perform
Serial Dilutions were performed,
Report al
SERIAL DILUTION ANALYSIS
For each matrix and results of the diluted sample analysis agreedundiluted analysis for analyte concentrations > 50x the IDL
ed for the following:
but analytical results did not agree within 10% for analyteconcentrations greater than 50x the IDL before dilution.
I results below that do not meet the required laboratory criteria for ICP serial dilution analysis.
MATRIX:
ELEMENT : IDL
AluminumBariumBerylliumCadmiumCalciumChromiumCobaltCopperIronLeadMagnesiumManganeseNickelPotassiumSilverSodiumVanadiumZinc
WxtOLSAMPU - ' .. sewAL ' .• - 'RESULT DILUTION %D ACTION
Actions apply to all samples of the same matrix.
ACTIONS:
1. Estimate (J) positive results if %D >15.
Form INT3-19
QSEA File: MA49F326.WB2 - 22
ICP SERIAL DILUTION VERIFICATION
Sample ID MAEP16L
ICP Analyte CALCIUM Lab Value 0.7
%D 25927 26109 / 25927 100 -0.70
Sample ID
ICP Analyte
MAEP16L
ZINC
%D 4.19 29.3
Lab Value 599.3
4.19 100 -599.28
FormlNT3-15A
QSEA File: MA49F326.WB2 - 23
SEA.,REGION IData Review Worksheets
XII. DETECTION LIMIT RESULTS
1. Instrument Detection Limits
_X Instrument Detection Limit results were present and found to be less than the ContractRequired Detection Limits.
IDLs were not included in the data package on Form XI.
IDLs were present, but the criteria was not met for the following elements:
2. Reporting Requirements
Were sample results on Form I reported down to the IDL notthe CRDL for all analytes? Yes X No
N/A Were sample results that were analyzed by ICP for Se, Tl,As, or Pb at least 5x IDL? Yes No
Were sample weights, volumes, and dilutions taken intoaccount when reporting detection limits on Form I? Yes X No
If NO,The reported results may be inaccurate. Make the necessary changes on the datasummary tables and request that the laboratory resubmit the corrected data.
FormWTJ.1*
QSEA File: MA49F326.WB2 - 24
\^f
„ REGION IData Review Worksheets
XIII. SAMPLE QUANTITATION
_X Sample results fall within the linear range for ICP and within the calibrated range for all otherparameters.
Sample results were beyond the linear range/calibration range of the instrument for the following"samples/elements:
In the space below, please show a minimum of one sample calculation per method:
ICP
100.00 / 100.00 X33196.00 (mg/L) X 1.00 33196
Sample ID = MACZ50, Calcium Lab Value = 33200 ug/L
FURNACE
N/A
MERCURY
-0.09 (mg/L) x 100.00 / 100.00 1.00 -0.0890
SamplelD = MAEP15 Lab Value = 0.2U
CYANIDE
-0.50 (mg/L) x 50.00 / 50.00 1.00 -0.5000
SamplelD = MAEPl5 Lab Value = 10.0U
For coil samples, the following equation may be necessary to convert raw data values (usually reported in ug/L)to actual sample concentrations (mg/kg):
The lab is required to use 1 gram sample (wet weight) to 200 ml.
Wet weight concentration =
digest cone, in (ug / L) x (200ml /1 gm) x (1L / 1000ml) x (1000gm / 1kg) x (1mg / 1000ug) = mg / kg
In addition, the sample results are converted to dry weight using the percent solids calculations:
(Wet weight cone / %solids) x 100 = final concentration, dry weight (mg / kg)
Form INTS-17
QSEA File: MA49F326.WB2 - 25