fiR30292U · quality assurance review analytical data soil, sediment and water samples roy f....
Transcript of fiR30292U · quality assurance review analytical data soil, sediment and water samples roy f....
QUALITY ASSURANCE REVIEWANALYTICAL DATA
SOIL, SEDIMENT AND WATER SAMPLESROY F. WESTON, INC. LABORATORY
(SAMPLES COLLECTED FROM NOVEMBER 1989 TO FEBRUARY 1990)
FEBRUARY 1991
VOLUME I
REMEDIAL INVESTIGATION/FEASIBILITY STUDYSTANDARD CHLORINE OF DELAWARE, INC.
DELAWARE CITY, DELAWARE
fiR30292U
STANDARD CHLORINECASE 9001L081
This quality assurance review is based upon a review of the datagenerated from two water and one soil samples collected on 01-05-90and analyzed by Roy F. Weston Lionville Analytical Laboratory forTCL Volatile and Semivolatile target compounds.
The reported analytical results are presented as a summary of thedata in Section II. All of the analytical data were examined todetermine the usability of the analytical results and also todetermine contractual compliance relative to the analyticalrequirements and deliverables specified in EPA's ContractLaboratory Program (CLP) protocol. Qualifier codes have beenassigned next to the results so that the data user can quicklyassess the qualitative and/or quantitative reliability of anyresults.
Details of this quality assurance review are presented in thenarrative section of this report under each fraction. This reportwas prepared to provide a critical review of the laboratoryanalyses and reported analytical results.
ftR302925
INFORMATION REGARDING DATA .___._,..
All data were reviewed according to CLP Functional Guidelines forEvaluating Organic Analyses. All data have been validated withregard to usability.
If you have any questions or comments on this data review, pleasecall Zohreh Hamid at (215)524-7360.
ATTACHMENTS
1. Attachment I - Glossary of Data Qualifier Codes.
2. Attachment II - Data Summary. This includes:
a) All positive results for the target analyteswith the qualifier codes, if applicable; and
b) All unusable detection limits (qualified "R") .
3, Attachment III - Re-submissions.
flR302926
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 9001L081PAGE 2 OF 5
EVALUATION BY FRACTION
I- Volatiles _
___ Holding Time___ Surrogate Recovery_2S__ MS/MSDx Blank___ GC/MS Tuningx Initial Calibrationx Continuing Calibration___ Compound ID (HSL, TIC)___ Standards___ Spectra Quality___ ChromatographyX Data Completeness
This portion of the case consisted of one soil and two watersamples which were analyzed according to CLP SOW 02/88 (Rev. 05/89)for TCL Volatile target compounds on 01-08r10-90.
The butanone response factor is less than the EPA QC limit of 0.05in the soil initial and continuing calibrations. The associatedguantitation limit is rejected and flagged "R" in the data summary.
Several compounds had %RSD and %D outside the 3d. and 25% EPA QClimits in the initial and continuing calibrations. Allcorresponding guantitation limits are qualified estimated, "UJ".
The soil blank contained common contaminant methylene chloride ata level less than 5x the CRQL and 1,1,1-trichloroethane at a levelless than the CRQL. The associated sample's positive result formethylene chloride was less than lOx the blank level and the resultfor 1,1,1-trichloroethane was less than 5x the blank contamination;therefore, for both compounds, the quantitation limit is adjustedto the value reported and is flagged "U". The blank also containstrichloroethene and 2-hexanone; however, the associated sample, SS-Tll-1-1 does not contain these compounds. Qualification was notapplied.
Sample SS-T11-1-1 required a 2.44 fold dilution due to a high levelof chlorobenzene- The dilution level seemed appropriate for thisanalyte.
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QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 9001L081PAGE 3 OF 5
Matrix spike/spike duplicate analyses were not performed with thisbatch of samples; therefore, the long term precision and accuracyof the analytical method cannot be evaluates*. No qualification isapplied on this basis alone.
The Form IV was missing for blank 90LVY008-MB1 and thetrichloroethene spectra was missing from sample SS-R19-1-4; bothsets of missing information are submitted with this report. Also,the incorrect Form V was submitted for the tune analyzed on 01-10-90 at 08:48; the corrected form is re-submitted.
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QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 9001L081PAGE 4 OF 5
EVALUATION BY FRACTION
II. Base/Heutral/Acids
___'m Holding Time___ Extraction Timex Surrogate Recoveryx BlankX MS/MSD___ GC/MS Tuning___ Initial Calibrationx Continuing Calibration___ Compound ID (HSL, TIC)___ Standards___ Spectra Quality___ Chromatography___ Data Completeness
This portion of the case consisted of one water and one soil samplewhich were analyzed according to CLP SOW 02/88 (Rev. 05/89) for TCLand client specified semivolatile target compounds on 02-02,06-90.
Sample SS-T-11-1-1 required a 111-fold dilution due to high levelsof target compounds. The If4-dichlorobenzene results still exceededthe calibration range; therefore, the sample was re-analyzed withinholding time at a 11100-fold dilution.. The more diluted sampleresult will be used for this compound. All other results come fromthe original analysis.
The soil blank contains 1,4-dichlorobenzene and di-n-butylphthalate(common contaminants) at levels less than the CRQL. The onlyassociated positive sample result is 1,4-dichlorobenzene in sampleSS-T-11-l-DL. The result is greater than 5x the blank level;therefore/ it is considered a true value.
Several compounds had %D in the continuing calibration exceed the25% EPA CLP QC limit. The associated positive results andquantitation limits are considered estimated and flagged "J andUJ».
The matrix spike/spike duplicate associated with this extractionbatch (90LE0032) is sample SS-T213-1-5 (9001L067-019). Seven of 22spike recoveries are outside the EPA CLP QC limits. The originalsample analysis contain several of these spiking compounds;therefore, the calculations of the spike recoveries are probablyattached. Also, three of 22 blank spike recoveries are outside QClimits. The long term precision and accuracy of the analyticalmethod cannot be evaluated. However, no qualification is appliedon this basis alone.
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QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 9001L081PAGE 5 OF 5
The surrogate recoveries for sample SS-T11-1-1 and its dilutionwere not able to be obtained due to the required dilution. Noqualification is applied.
The following nine client specified compounds were library searchedand several were detected in these samples:
AnilineN-nitrosodiphenylamineBenzidine1,2,3-Trichlorobenzene1,3,5-TrichlorobenzenePentachlorobenzenel-chloro-3 - nitrobenzene1,2,4,5-tetrachlorobenzene1,2,3,4-tetrachlorobenzene
•ftfc
* GLOSSARY OF DATA QUALIFIERS
CODES RELATING TO IDENTIFICATION
(confidence concerning presence or absence of compounds)
0 = NOT DETECTED, SUBSTANTIALLY ABOVE THE LEVELREPORTED IN LABORATORY OR FIELD BLANKS.
R =-- UNRELIABLE RESULT. ANALYTE MAY OR MAY NOT BEPRESENT IN THE SAMPLE. SUPPORTING DATANECESSARY TO CONFIRM RESULT.
N = NEGATED COMPOUND WAS CONSIDERED AS NOTPRESENT IN THE SAMPLE.
(NO CODE) = CONFIRMED IDENTIFICATION
CODES RELATING TO QUANTITATION
(can be used for both positive results and sample guantitationlimits):
J = . - - : ANALYTE PRESENT. REPORTED VALUE MAY NOT BEACCURATE OR PRECISE.
UJ = THE REPORTED QUANTITATION LIMITS AREQUALIFIED ESTIMATED.
OTHER CODES
NO ANALYTICAL RESULT.
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5R302938
4Af VOLATILE METHOD BLANK SUMMARY
Lab Vaae: Rov F, Weaton, Inc. Contract! 2267-09*02-0000
Ca«e Ho.: STANDARD CHLORINE______
Lab File ID: Y011003_____ Lab Sample IDi 90LVYQ08-MB1
I Date Analyzed: 01/10/90 Time Analyzed: 09 S 9
| Matrix: (Soil/Hater) SOIL Level: (lovr/med) MED
Instrument ID: 5100Y____
THIS METHOD BLANK APPLIES TO THE FOLLOWING SAMPLES, MS AND M5D:
CLIENT LA LA TIMESAMPLE NO. j SAMPLE ID FILE ID ANALYZED
OISS-TII-I-I (9001L081-029 | Y01100B | 1606
COMMENTS;
page 1 of 1 PORM IV VOA 5/88 Rev.
flR3029UO
IVOLATILE ORGANIC GC/MS TONING AND MASSCALIBRATION - BROMOFLUOROBENZENE (BFB)
Lab Name: Sov F- Westop* Inc. Contract: 2267-09-02-0000
Case KO.J STAND ASP CSLQRIN1
O'l
* Lab File ID: Y011QQ1 * BFB Injection Date: 01/10/90
• instrument IDt S1QQY BFB Injection Time: 848
Matrix* (soil/water) SOIL Level: (low/med) MED Column: (pack/cap) PACKiSO759596173174175176177
1ION ABUNDANCE CRITERIA
15.0 - 40.0% of nass 9530.0 - 60.0% of mass 95Base peak, 100% relative abundance5.0 - 9.0% of mass 95Less than 2.0% of mass 174Greater than 50.0% of mass 955.0 - 9.0% of mass 174Greater than 95.0% but less than 101.0% of mass 1745.0 - 9.0% of mass 176
'
% RELATIVEABUNDANCE
25.447.5100.08.40.0{ 0.0)199.17.7{ 7.8)194. 8( 95.7)17.6( 8.0)2
1-Value is % mass 174 2-Value is % mass 176
THIS TUNS APPLIES TO THE FOLLOWING SAMPLES, MS, MSD, BLANKS, AND STANDARDS:
14
CLIENT | LABSAMPLE NO. | SAMPLE ID
V3TD050 ""~ | VSTD050VBLKLVX068-ME1 | 90LVX008-MB133-T11-1-1 | 9001L081-O29
1111
111
1
1
II
1
LABFILE ID
Y011002X011003Y011008
DATEANALYZED
01/10/9001/10/9001/10/90
.
t
TIMEANALYZED
090709591606
page l of l FORM v VOA 1/87 Rev,
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III
STANDARD CHLORXBECASE 9001L067 AND 9001LOS1 (PESTICIDE/PCB OHI.T)
This quality assurance review is based upon a review of the datagenerated from two water and four soil samples collected on01-04-90 for TCL Volatile, Semivolatile, and Pesticide/PCB targetcompounds for Case 9001L067 and one water and one soil samplecollected on 01-05-90 for Pesticide/PCB target compounds only forCase 9001L081. These samples vere analyzed by Roy F. WestonLionville Analytical laboratory.
The reported analytical results are presented as a summary of thedata in Section II. All of the analytical data were examined todetermine the usability of the analytical results and also todetermine contractual compliance relative to the analyticalrequirements and deliverables specified in EPAf s ContractLaboratory Program (CLP) protocol. Qualifier codes have beenassigned next to the results so that the data user can quicklyassess the qualitative and/or quantitative reliability of anyresults.
Details of this quality assurance review are presented in thenarrative section of this report under each fraction. This reportwas prepared to provide a critical review of the laboratoryanalyses and reported analytical results. ^
INFORMATION REGARDING DATA
All data were reviewed according to CLP Functional Guidelines forEvaluating Organic Analyses. All data have been validated withregard to usability.
If you have any questions or comments on this data review, pleasecall Zohreh Hamid at (215)524-7360.
ATTACHMENTS
1. Attachment I - Glossary of Data Qualifier Codes.
2. Attachment II - Data Summary. This includes:
a) All positive results for the target analyteswith the qualifier codes, if applicable; and
b) All unusable detection limits (qualified "R") .
3. Attachment III - Re-submissions.
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 9001L067CASE 9001L081 PEST/PCBPAGE 2 OF 7
EVALUATION BY FRACTION
I. Volatiles
___ Holding Timex Surrogate Recovery
____ MS/MSDx_ Blank
___ GC/MS Tuningx Initial Calibrationx Continuing Calibration
___ Compound ID (HSL, TIC)x Standards
___ Spectra Quality___ Chromatographyx Data Completeness
This portion of the case consisted of two water samples and foursoil samples which were analyzed according to CLP SOW 02/88 (Rev.05/89) for TCL Volatile target compounds on 01-08,09,10-90
The following samples had surrogate recoveries exceed the EPA CLPQC limits and internal standard areas were below the EPA QC limits.Sample results may be biased high.
Sample Surrogate Internal Standards
SS-T41-1-1/MS/MSD ** 1,2-Dichloroethane Chlorobenzene1,4-DichlorobenseneBromochloromethane
SS-T23-1-1 * TolueneBromofluorobenzene Chlorobenzene
SS-T-23-1-2 * TolueneBromofluorobenzene Chlorobenzene
** This sample and its associated QC samples were not re-analyzed; therefore, all positive results andguantitation limits are considered estimated "J and UJ",respectively.
* The samples were re-analyzed within holding time at alower level dilution with no surrogate or internalstandard outliers; therefore, the representative sampleresults should come from the re-analysis.
The response factors for 2-butanone and 4-methyl-2-pentanone werebelow the EPA QC limit of 0.05 in the initial and continuingcalibrations. All associated guantitation limits are rejected.
r\
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 9001L067CASE 9001L081 PEST/PCBPAGE 3 OF 7
Sample SS-T23-1-5 was re-analyzed within holding time at a lowerdilution due to the concentrations of benzene and chlorobenzene.The more diluted original analysis is not to be used. Therepresentative results come from the less diluted re-analysisresults.
Several compounds had %RSD and %D for initial and continuingcalibrations exceed the 30 and 25% EPA QC limits. Allcorresponding positive results and guantitation limits arequalified estimated.
The laboratory blanks contain methylene chloride and acetone(common contaminants) at levels less than 5x the CRQL and severalother target compounds at levels less than the CRQL. Allassociated common contaminant positive results are less than lOxthe blank level and all other corresponding target compoundpositive results are less than 5x the blank contamination,therefore, the guantitation limits for these compounds are adjustedto the level of the value reported and are flagged "U" in the datasummary.
There was a discrepancy between the Form V and mass spectra/listfor the tune analyzed on 02-09-90 at 14:10. The corrected Form Vis re-submitted. Also, the Form VI on the calibration on 01-05-90did not correspond to the raw data. Corrected Form VI and Form VIIare resubmitted.
The package was missing Form VIII's for VBLKLVX005-MB1, VBLKLVX007-MB1, VBLKLVY008-MB1, SS-723-1-1 RE, SS-T23-1-2 RE, and SS-T23-1-5.The Form VIII's are submitted with this report.
The % relative abundance m/e = 176 for the tune on 11-14-89 at 7:19was not completely calculated. The corrected Form V is attached.Also, sample SS-T41-1-4TBDL was -removed from the Form V on 01-09-90at 16:01. This was a mis-print and the corrected form is re-submitted.
Dichlorobenzenes were reported as tentatively identified compoundsin several samples. These compounds should be reported in the BNAfraction of the sample.
All matrix spike recoveries were within EPA QC limits.
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 9001L067CASE 9001L081 PEST/PCBPAGE 4 OF 7
EVJLLUATION BY FRACTION
II. Base/Neutral/Acids
___ Holding Time___ Extraction Time___ Surrogate Recoveryx Blank
__£_ MS/MSD___ GC/MS Tuning___ Initial Calibrationx Continuing Calibration___ Compound ID (HSL, TIC)___ Standards___ Spectra Quality___ Chromatography___ Data Completeness
This portion of the case consisted of one water and four soilsamples which were analyzed according to CLP SOW 02/88 (Rev. 05/89)for TCL and client specified semivolatile target compounds on 02-02,06-90.
The soil blank contains 1,4-dichlorobenzene at levels greater than5x the blank level; therefore, these results are considered truevalues* The di-n-butylphthalate positive sample results are lessthan lOx the blank contamination. These samples have thequantitation limits adjusted to the value reported and are flagged"U" in the data summary.
Several compounds had %D in the continuing calibrations exceed the25% EPA CLP QC limit. All corresponding guantitation limits arequalified estimated and flagged "UJ11.
Seven of twenty-two matrix spike recoveries are outside EPA CLP QClimits. The original sample analysis contain several of these samespiking compounds; therefore, the calculations of the spikerecoveries were probably affected. Also, three of twenty-two blankspike recoveries are outside EPA CLP QC limits. A reliableevaluation of the long term precision and accuracy of theanalytical method cannot be done. However, no qualification isapplied on this basis alone.
I1
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 9001L067CASE 9001L081 PEST/PCBPAGE 5 OF 7
The following nine client specified compounds were library searchedand several were detected in these samples:
AnilineN-nitrosodiphenylamineBenzidine1,2,3-Trichlorobenzene1,3,5-TrichlorobenzenePentachlorobenzenel-chloro-3-nitrobenzene
~1,2,4,5-tetrachlorobenzene1,2,3,4-tetrachlorobenzene
AR302950
II QA ORGANIC DATA REVIEW
STANDARD CHLORINECASE 9001L067
I CASE 9001L081 PEST/PCBPAGE 6 OF 7
I EVMitJMIOH BY FRACTION
III. Pesticides/PCB
Holding TimeExtraction TimeSurrogate RecoveryMS/MSDBlankLinearity CalibrationDDT/Endrin DegradationAnalytical SequenceDEC Retention TimeContinuing CalibrationRetention Time WindowStandardsChromatographyHSL CompoundsData Completeness
These portions of the cases consisted of two water and five soilsamples which were" analyzed for TCL Pesticide/PCB targetcompounds on 02-03,04-90.
The following soil samples required dilution due to high levels ofnon-target compounds:
Sample Dilution Factor
SS-T23-1-1 2SS-T24-1-2 2SS-T23-1-5 5SS-T11-1-1 20
The matrix spike/spike duplicate recoveries in sample SS-T23-1-5for gamma-BHC (I/I) and 4,4'-DDT (—/I) were outside the QC limits.The original sample and QC samples contain higher levels of non-target compounds that probably interfere with the matrix spikerecoveries. These spike compounds were not detected in thesamples; therefore, no qualification is applied. All blank spikerecoveries were within QC limits.
AR30295
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 9001L067CASE 9001L081 PEST/PCBPAGE 7 OF 7
All of the %D for IND A on 02-03-90 at 19:47 on the primary columnand IND B on 02-04-90 at 04:09 on the confirmation column exceededthe 15% and 20% requirement limits. Several other %D exceeded the20% limits for the confirmation column for the remainder of theindividual A and B mixes. However, most compounds with theexception of dieldrin, were not detected in the samples. Thedieldrin result in sample SS-T41-1-1 is considered estimated.There is no impact to the rest of the data.
Many retention time criteria on both columns were outside theestablished retention time windows for compounds analyzed prior tothe samples. These compounds were not detected in the samples;therefore, there is no impact to the data.
The laboratory reported that the column flow was not equilibratedwhen the analysis was started and that there was a slight shift inretention times on both columns. This was consistent through therun and the retention time windows were extended to coincide withthe shift. The validator agrees with this statement and the datahas been qualified in reference to the problems mentionedpreviously in this report.
&R302952
GLOSSARY OF DATA QUALIFIERS
COPES RELATING TO IDENTIFICATION
(confidence concerning presence or absence of compounds)
0 = NOT DETECTED, SUBSTANTIALLY ABOVE THE LEVELREPORTED IN LABORATORY OR FIELD BLANKS.
R = UNRELIABLE RESULT. ANALYTE MAY OR HAY NOT BEPRESENT IN THE SAMPLE. SUPPORTING DATANECESSARY TO CONFIRM RESULT.
N = NEGATED COMPOUND WAS CONSIDERED AS NOTPRESENT IN THE SAMPLE.
(NO CODE) = CONFIRMED IDENTIFICATION
CODES RELATING TO QUANTITATION , .
(can be used for both positive results and sample guantitationlimits):
J = - ANALYTE PRESENT. REPORTED VALUE MAY NOT BEACCURATE OR PRECISE.
UJ = THE REPORTED QUANTITATION LIMITS AREQUALIFIED ESTIMATED.
OTHER CODES
NO ANALYTICAL RESULT.
BR30295U
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VOIATILB ORGANIC GC/HS TONING AMD MASSCALIBRATION - BROMOFLUOROBENZENX (BFB)
Lab Xame: Roy F. Wagton* Inc. Contract: 2267*09-02-0000
CAM *».: STANDARD CHLORINE______
LAb File IDJ Y011001 „ BFB Injection Date: 01/10/9O
Instrument IDt 5100Y BPB Injection Time: 848
Matrix: (soil/water) SO.II... Level: (low/mod) jgp_ Column: (pack/cap) PACK
m/e
50759596173174175176177
ION ABUNDANCE CRITERIA
15.0 - 40.0% of mass 9530.0 - 60.0% of mass 95Base peak, 100% relative abundance5.0 - 9.0% of masB 95Less than 2.0% of mass 174Greater than 50.0% of mass 955.0 - 9.0% of mass 174Greater than 95.0% but less than 101.0% of mass 1745.0 - 9.0% of mass 176
/
% RELATIVEABUNDANCE
25.447.5100.08.40.0( 0.0)199.17.7( 7.8)194. 8( 95.7)17.6( 8.0)2
l-Value is % mass 174 2-Value is % mass 176
THIS TONE APPLIES TO THE FOLLOWING SAMPLES, MS, BSD, BLANKS, AND STANDARDS:
02 |03|04 |05 I06 I07 j08 I09 |10|HI12|13 |14|15 |16|17 |18119 |201
CLIENTSAKPLE NO.
VSTD050VBLKLVYOOB-MB1SS-T2 3-1-1SS-T23-1-2SS-T23-1-5
LAB | LABSAMPLE ID j FILE ID
£3S=se5=SS=Ei=ds:=e:=e j SKSSCS=SKSS =SC
vsTDOBO | roiiooa90LVY008-MB1 j Y0110039001L067-017 j Y0110059001L067-018 | Y0110069001L067-019 j Y011007
1111111I11111111
DATEANALYZEDssxe2S=s:B=Ss
01/10/9001/10/9001/10/9001/10/9001/10/90
TIMEANALYZED
09070959115412351316
page 1 of 1 FORM V VOA 1/87 Rev.
5AVOLATILE .ORGAKIC 6C/KS TUNING AMD K&SS 028CALIBRATION - BRQHOFLTORQBBNZENB (BFB)
Lab Name: Rov F* Weaton, Inc. Contract: 2267-09-02-OOOO
Cat* Ho.I STANDARD CHLORINE______
Lab File ID: AK19&1 , BFB Injection Date: 1/09/90
In»trua«nt IDi S*-MSD K BFB Injection Time: 1601
Matrix:(soil/water) WATER L«vel:(low/mad) Ifig Columns (pack/cap) GAP
m/e
SO759596173174175176177
ION ABUNDANCE CRITERIA
15.0 - 40.0% of" maim 9530.0 - €0.0% of mass 95Baie peak, 100% relative abundance5.0 - 9.0% of mass 95Le«« than 2.0% of mass 174Greater than 50.0% of mass 955.0 - 9.0% of mass 174Greater than 95.0% but less than 101.0% of mass 1745.0 - 9.0% of masiTl76
-
% RELATIVEABUNDANCE
32.556.5100.07.20.0(65.73.9(64. 7(3.5(
0.0)1
6.0)198.5)15.5)2
1-Value is % mass 174 2-Value is % mass 176
THIS TONE APPLIES TO THE FOLLOWING SAMPLES, MS, MSD, BLANKS, AND STANDARDS:
0102030405060708091011121314151617131920
CLIENT | LABSAMPLE NO. j SAMPLE ID
VSTDSO | VSTD50VBLKLVK004-KB1 j 90LVX004-MB1SS-T41-1-3 FB j 9001L067-00133-T41-1-4 TBBL | P001L067-003
111111111I111I111
LABFILE ID
AK1902AK1903.AK1904.
DATEANALYZED
01/09/9001/09/9001/09/90
1
TIMEANALYZED
164417431855
1931 6\
page 1 of 1 FORM V VGA 1/87 Rev.
AR302965
J VOLATILE ORGANIC GC/MS TURING AND MASS 030CALIBRATION - BROMOFUTOROBBNZENK (BFB)
m Lab Name: Rov F, Weaton, Inc. Contract: 2267-09*02-0000
" case mo.t STANDARD CHLORINE
iii
^Lab File IDs AgS801 BFB Injection Date* 11/14/69
Instrument IDs g»-MSD- X BFB Injection «J»J 719
Matrix:(»oil/water) SOIL Leveli (low/mod) LOW Column; (pack/cap) CAP
11 50I 75I 951 96| 173| 174I 175| 176| 1771 ____
1ION ABUNDANCE CRITERIA j
15.0 - 40.0% of ma»« 95 f30.0 - 60.0% of mass 95 fBase peak, 100% relative abundance I5.0 * 9.0% of mass 95 fLess than 2*0% of mas a 174 IGreater than 50.0% of mass 95 15.0 - 9.0% of mass 174 IGreater than 95.0% but leas than 101.0% of mass 174 15.0 - 9.0% of mass 176 j
1
% RELATIVEABUNDANCE
18.950.1100.06.70.0( 0.0)177.35,5{ 7.2)1|77. 4( 100. 1 )15.7( 7.4)2 7 ••*•"
1-Value is % mass 174 2-Value is % masa 176
THIS TONE APPLIES TO THE FOLLOWING SAMPLES, MS, MSD, BLANKS, AND STANDARDS:
| CLIENT j US j LAB j DATE j TIMESAMPLE NO. SAMPLE ID PILE.ID ANALYZED ANALYZED
01| VSTD20 j VSTD20 j AXBE02 j 11/14/89 | 081702 j VSTD50 j VSTD50 j AXBE03 | 11/14/89 | 0849031 VSTD100 j VSTD100 | AXBE04 j 11/14/89 j 0920041 VSTD150 j VSTD150 j AXBE05 | 11/14/89 j 095205j VSTD200 | VSTD200 j AXBE06 | 11/14/89 | 1024°6| I ! I I0 7 | I I I !08| | | ||09| | | f |10) I I I IH I ! I I I12| | | | |13| I I I I1 4 | f i l l1 5 1 t i l l1 6 1 I I I I -171 I I I I18| I I I I191 I I I I201 1 I I f
age 1 of 1 FORM V VOA 1/87 Rev.
4R3Q2966
II
I
6AVOLATILE OBGAKICS 1NTITIAL CALIBRATION DATA
Lab name: Rov r. weaton. Inc. .' Contract: 2267-09-02*0000
Caie Ho.: ffTjUIDARD CHLORIKB______ RfW Lot: 90O1L067
Instrument ID: HP-KSD K Calibration Date(«); 01/05/90 01/05/90
Hatrix:(soil/water) IRTIR Level: (low/n»d) LOW Column: (pack/cap) CAP
Kin RRF for SPCC{#) « 0*300 (0.250 for Bromoform) ' Max %RSD for CCC(*) * 30.0%
|LAB FILS ID: RRF20 » AK1503[RRF100« AKX5Q4 RRT150- A1U50S
1COMPOUND (BRF20
Chloromethane * 0.564| Bromocve thane | 1.273(Vinyl Chloride * 0.870jChloroethane 1 0.638(Methylene Chloride i 1.592(Acetone 1 0.277Carbon Dimilfide 1 3.2341.1-Dichloroethene * 1.2561,1-Dichloroethane # 0.8031,2-Dichloroethene (total) ___ | 1.432[Chloroform * 4.3201,2-Dichloroethane | 0.8252-Butanone | 0.0601.1.1-Trichloroethane | 5.076(Carbon Tetrachloride | 2.950|Vinyl Acetate 1 48.55Bromodichloromethane | 1 . 0611 , 2-Dichloropropane * 0 . 349ci«-l, 3-Dichloropropene | 0.540[Trichloroethene 1 0.540| Dibromochloromethane | 0.991|lP1.2~Trichloroethane i 0.416Benzene , | 0.771Tran«-l,3-Dichloropropene ____ | 0.976Bromoform, ,„ „ „ ,.,..„„.,., , * 1.2194-KethYl-2-pentanone | 0.0102-Hexanone | 0.339|T*trachloroethene | 0.8051,1,2,2-Tetrachloroethane ____ # 0.622(Toluene * O.749(Chlorobenzene t 1.050Ethvlbenzene * 0.453Stvrene | 0.929|Xvlene ( total} 1 1.630
Toluene-d8 1 1.587Bromof luorobenrene | 1 . 5 12l,2-Dichloroethane-d4 | 0.827
1
—
1RRF50 |
0.471 |1.066 |0.666 |0.5481.3180.187 |2.566 |1.2020.8091.2843.8630.7430.1454.3395.0940.8191.0280.3110.5150.5460.9710.4270.7420.9361.2170.0210.3001.0280.6450.6781.0190.4320.9190.282
1.1781.2250.646
RRF5CRRT2C
RRF100
0.4671.1480.6610.5251.054
. 0.147" 2.7791.1250.7091.1063.4920.6740.0844.0294.7200.4390.9120.2840.4420.4530.8120.3720.6470.8460.9680.0140.2630.8660.5220.5940.8560.3740.7491.354
1.2331.1780.678
» « AK1502»0- AK1506
1RRF150 |RRF200
0.516 | 0.4761.202 | 1.1440.719 | 0.6950.560 | 0.5381.143 | 1.1000.219 | 0.1743.050 | 2.9841.228 | 1.1820.744 | 0.7141.222 | 1.1843.813 | 3.6210.725 | 0.6680.101 | 0.1084.368 1 4.1194.972 | 4.7840.486 | 0.4121.010 | 0.8790.310 | 0.2950.500 | 0.5330.499 | 0.4640.909 | 0.8670.404 | 0.3940.713 | 0.6600.923 | 0.8381.099 1 1.0650.020 | 0.0200.288 1 0.2670.732 | 0.7600.603 | 0.5800.662 | 0.5980.960 | 0.9360.416 | 0.3940.877 | 0.8311.484 | 1.442
1.290 1 1.1951.286 | 1.1740.710 | 0.643
1
RR?
0.4991.1670.7220.5621.2410.2012.9231.1980.7561.2463.8220.7270.1004.3864.50410.140.9780.3100,5060.5000.9100.4020.7070.9041.1140.0170.2910.8380.5950.6560.9640.4140.8611.238
1.2971.2750.701
% 1RSD |«,«|8.4*6.6|11.9*7.9|17.7|24,818.8)4.1*6.3*«"
31.619.4|19.6|
211. 8|8.0{7.9*7.7|8.5|e.i|5.2]7.5)6.6[9.6*27.0|10.6)14. 0|8. Of9.7*7.8*7.5*8.5|43. 9[
"41iJBl10.8]
iFORM VI VOA 01/89 Rev.
AR302967
7AVOLATILE CONTINUING CALIBRATION CHKOC
Lab Names Rov F. Weston. Inc, Contracti 2267-09*02-0000
Case NO. t STANDARD CHLORINE______ RPW Lot: 9001L067
Instrument ID: HP-MSP. K Calibration Data: 01/09/90 Time: 1644
Lab Fll» ID: AK1902 Init. Calib. Date(«): 01/05/90 01/05/90
Matrix {(soil/water) WATER levels (low/med) |£W Column: (pack/cap) CAP
Min RRF50 for SPCC(f) - 0.300 (0.250 for Bromof orm Max %D for CCC{») - 25.0%
1j COMPOUND
j Chloromethane| Bromomethane| Vinvl Chloride| Chloroethane ,[Methylene Chloride| Acetone[Carbon Bisulfide| 1 r 1-Dichloroethene| 1 . 1-Dichloroethane|l,2-Dichloroethene (total)| Chloroform1 1 , 2-Dichloroethane1 2-Butanone1 1 , 1 , 1-Trichloroethane(Carbon Tetrachloride| Vinvl Acetate| Bromodichloromethane| 1, 2-Dichloropropane| cis-1 , 3-Dichloropropene| Trichloroethene| D ibromochl or ome thane| 1 , 1 , 2 -Tr ichloroethane| Benzene| Trana-1, 3-Dichloropropene*| Bromof orm| 4-Methyl-2-pentanone| 2-Hexanone| Tetrachloroethene11,1,2, 2-Tetrachloroethane| Toluene| ChlorobenzenelEthvlbenzene1 styrenef Xvlene ( total )1 s
j Toluene-d8| Bromof luorobenzene| 1, 2-Dichloroethane-d41
| __j RRF
t 0.499| 1.167* 0.722| 0.562| 1.241| 0.201| 2.923* 1.1*98# 0.756| 1.246* 3.822| 0.727| 0.100| 4.3861 4.504| 10.14| 0.978* 0,310| 0.506| 0.5001 0.910| 0.402| 0.707| 0.904* 1.1141 0.017| 0.291| 0.838* 0.595* 0.656t 0.964* 0.414| 0.861| 1.238
1 1.297| 1.275! 0.7011
RRF50
0.5101.2520.7260.5981.2350.2212.7521.1690.8091.2784.0490.7890.1154.8225.4610.7181.0860.2900.5060.5030.9800.4290.6970.9821.1600.0190.3000.7020.6120.6860.9670.4200.8471.549
1.3791.3640.760
%D
-2.3 '•-7.3-0.6 *-6.40.5
-10.15.92.4 *
-7.0 1-2.6-5.9 *-8.5
-14.9-9.9
-21.392.9
-11.06.40.1
-0.6-7.7-6.61.5
-8.6-4.1-9.6-3.016.2-2.8-4.5-0.3-1.51.6
-25.2
-6.3-7.0-8.4
FORM VII VOA 5/88 Rev.
AR302968
r 7AVOLATILE CONTINUING CALIBRATION CHECK
Lab Kaaa-i RQV f» Wyatonr Inc, Contract: 2267-09-02-0000
Caee Ho.: 8TAKPAKP CHLQBI^g_____ RFH Lot: 9001LQ67
In«tru»«nt ID: HP-MSD K Calibration Data: 01/10/90 Tiafts 1644
Lab Ul« IDs AK1A02 Init. Calib. Dat*(»)t 01/05/90 01/05/90
Matrix: {«oil/wat»r} BATKR Lavel: (low/med) LOW Column: (pack/cap) CAP
Kin BRFSO for SPCC(f) * 0*300 (0.250 for Bromoform Max %D for CCC(*) - 25.0%
i
ij COKPOOTD
j Chloromethane ,„ „ , .._| Bromomethane(Vinyl Chloride| Chloroathana , .iMafchylana Chloride| Acetone[Carbon Dimulf ids ,„,„._ ,| lf l-Dichloroethene , , ,,„ „. „1 1 , l-Dlchloro*thane|if2-Diehloro«th«n« (totals. . „| Chloroform| lf 2-Dichloroethane| 2-Eutanon«| 1 f 1 f 1-Trichloroethane| Carbon Tetrachloride(Vinyl Ac*tate[Bromadichloron»thane|lf2-Dichloropropane , ,.,..| ci«-l r 3-Dichloropropene| Triehloroethene|Dibromochloromethane , , , ,„ „ „1 1 f 1 f 2-Trichloroethane| Benzene| Trans-1 . 3-Dichloropropeno| Brooof om1 4-K«thvl-2-r>entanone| 2-Heaanone| Tetrachloroethene| 1 t 1 , 2 , 2-Tetrachloroethane| Toluene| Chlorobenrene| Ethylbanrene| Stvrene|Xylene { total i1 m
| Toluene-d8| Bromof luorobenzene1 1 , 2-Bichloroethane-d4I
1 __ I1 *s* If 0.499| 1.167* 0.722| 0.562| 1.241| 0.201| 2.923* 1.1*8* 0.756| 1.246* 3.B22| 0.727| 0.100| 4.386| 4.504| 10.14| 0.978* 0.310| 0.506| 0.500| 0.910| 0.402| 0.707| 0.904# 1.1141 0.017| 0.291| 0.838i 0.595* 0.656i 0.964* 0.4141 0.861| 1.238
| 1.2971 1.275| 0.7011
ra?500.4911.0690.6940.5791.1050.1952.6301.0920.6981.2133.4810.7070.0953.8674.4030.3940.9210.3060.4290.5980.9170.4380.7270.8241.1920.0270.3830.8350.5570.6290.9580.4090.8611.448
1.2261.2240.693
%D
1.78.43.9-3.111.03.210.08.87.62.78.92.75.311.82.296.15.81.315.3-19.7-0.8-8.9-2.88.8-7.0-56.1-31.50.36.44.10.61.10.0
-17.0
5.44.01. 1
FOHM VII VOA 5/88 Rev.
flR302969
8AVOLATILE INTERNAL STANDARD ARXA SUMMARY
Lab Name: Rov F. Weaton. Inc. Contracts 2267-09-02-0000
Ca*e No.s STANDARD CHLORINE______ RPW Lots 9001L067
Lab File ID (Standard).s A3C1802 Data Analyzed? 01/08/90
Instrument IDs HP-MSD J. Time Analyzeds 0825
Matrix: (soil/water) SEDIMENT Level:(low/med) fcpw Columns (pack/cap) CAP
01020304
| ISl(BCH) || AREA #| RTI |
12 HOUR STD | 25035 | 5.7S
UPPER LIMIT | 50070 | 6.25
LOWER LIMIT | 12518 | 5.25f i
CLIENT SAMPLE | |NO. | |
SS-T23-1-1 | 15174 | 5.77SS-T23-1-2 | 14361 | 5.79SS-T23-1-5 | 16737 | 5.74VBLKLVX005-MB1 | 21573 | 5.77
1 1
IS2(DFB)AREA i
103712
207424
51856
:
62617586196448286600
RT
8.46
8.96
7.96
8.488.508.488.48
IS3(CBZ)AREA *
81193
162386
40597
40039*34640*4838968876
RT
15.07......15.57
mmmmmx
14.57
15.1215.1015.0815.06
IS1 (BCM) * Bromochloromethane UPPER LIMIT « + 100%IS2 (DFB) « l,4-Difluorob©nzene of internal standard area.IS3 (CBZ) «' 'Chlorobenzene-dS LOWER LIMIT = - 50%
of internal standard area.
f Column uaed to flag internal standard area values with an asterisk
page 1 of 1 FORM VIII VOA 5/88 Rev.
fiR3Q2970
8AVOLATILE IKTKRNAL STANDARD AREA SUMMARY
Lab Mam*i Roy F» Weston, Inc. Contract: 2267*09*02*0000
Case Mo.: STANDARD C iOitllTl______ RTW Lot: 9001L067
Lab File ID (Standard).! A3C1A02 Data Analyzed: 01/10/90
Instrument ID: HP-MSD 3C Time Analyzedt 1404
Matrixi(«oil/water) SS3DSHT Level: (low/mad) LOW Columns (pack/cap) CAP
01020304
\ ISl(BCH)\ AREA *
12 HOUR STD \ 21551
UPPER LIMIT 1 43102ut»*»UJtJum«Lmjit»m*_*«- ^^rwmwr j *»ww«t»«t«»mm
LOWER LIMIT | 10776
CLIENT SAMPLE |NO. |
SS-T41-1-1 1 11675SS-T41-1-1MS | 11135SS-T41-1-1MSD | 9916*VBLKLV3C007-MB1 j 18633
1
RT
5.75
6.25
5.25C»»XK>
„««
5.765.765.795.79
IS2(DFB)AREA f
88730
177460
44365
*&*«KKXKX
4454043918*37360*77176
RT
8.46
8.96
7.96
8.458.458.488.48
IS3(CBZ)AREA t
71698
143396
35849«««,«„.
mmmmmmm~mmm
32439*33789*27915*61407
RT
15.08
15.58
14.58
15.0715.0815.0615.08
IS1 (BCK) - Bromochloromethane UPPER LIMIT - + 100*IS2 (DFB) * 1,4-Difluorobenzene of internal standard area.IS3 (CBZ) « Chlorobenzene-dB LOWER LIMIT » - 50%
of internal standard area.
t Column used to flag internal standard area values with an asterisk
page 1 of 1 FORM VIII VOA 5/88 Rev.
AR30297I
1
8AVOLATILE INTERNAL STANDARD ARSA SUMMARY
Lab Name: Roy g, Weston. Inc. Contractt 2267-09-02-OOOO
Case Mo.: STANDARD CHLORINg______ RFW Lot: 90011.067
Lab File ID (Standard): ¥011002 Date Analyzedi 01/10/90
Instrument ID: 5100Y Tine Analyzed: 0907
Matrix: (soil/water) SSPDfflNT Levels (low/med) IBP Column: (pack/cap) PACK
01020304
12 BOOR STD
DPPER LIMIT
LOWER LIMIT
CLIENT SAMPLENO.
SS-T23-1-1SS-T23-1-2SS-T23-1-5VBLKLVY008-MB1
ISl(BGM)AREA t
73405
146810«-»«-*«««»
36703
68912676697159772895
| IS2(DFB)RT f ARKA f
4.77| 266641
5.27| 533282»*»«> I »«3:M»s,»
4.27J 133321
ii4.33 | 2725624.37J 2622934.37| 2629914.73) 262340
RT
13.37
13.87—————12.87
13.3013.3713.3313.37
IS3(CBZ)AREA *
235077
470154
117539
241422233126236182234568
IRT |
17.83}
18.33|
17.331««..(
11
17.83|17.90|17.87J17.87|
IS1 (BCM) * Brooochloromethane UPPER LIMIT - + 100%IS2 (DFB) •= 1,4-Difluorobenzene of internal standard area.IS3 (CBZ) * Chlorobenrene-d5 LOWER LIMIT * - 50%
of internal standard area.
# Column used to flag internal standard area values with an asterisk
page 1 of 1 FORM VIII VOA 5/88 Rev.
flR302972
STANDARD CHLORISBCASE 9001L127
This quality assurance review is based upon a review of the datagenerated from two water and four soil samples collected on01-09,10-90 and analyzed by Roy F. Weston Lionville AnalyticalLaboratory for TCL Volatile, Semivolatile, and Pesticide/PCB targetcompounds.
The reported analytical results are presented as a summary of thedata in Section II. All of the analytical data were examined todetermine the usability of the analytical results and also todetermine contractual compliance relative to the analyticalrequirements and deliverables specified in EPA's ContractLaboratory Program (CLP) protocol. Qualifier codes have beenassigned next to the results so that the data user can quicklyassess the qualitative and/or quantitative reliability of anyresults.
Details of this quality assurance review are presented in thenarrative section of this report under each fraction. This reportwas prepared to provide a critical review of _ the laboratoryanalyses and reported analytical results.
AR302973
INFORMATION REGARDING DATA
All data were reviewed according to CLP Functional Guidelines forEvaluating Organic Analyses. All data have been validated withregard to usability.
If you have any questions or comments on this data review, pleasecall Zohreh Hamid at (215)524-7360.
ATTACHMENTS
1. Attachment I - Glossary of Data Qualifier Codes.
2. Attachment II - Data Summary. This includes:
a) All positive results for the target analyteswith the qualifier codes, if applicable; and
b) All unusable detection limits (qualified "R") .
3. Attachment III - Re-submissions.
III
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 9001L127PAGE 2 OF 7
EVALUATION BY FRACTION
I- Volatiles
___ Holding Timex Surrogate Recoveryx MS/MSDx Blank___ GC/MS Tuningx Initial Calibrationx Continuing Calibration___ Compound ID (HSL, TIC)___ Standards ____ Spectra Quality :""___ Chromatographyx Data completeness
This portion of the case consisted of two water and four soilsamples which were analyzed according to CLP SOW 02/88 (Rev. 05/89)for TCL Volatile target compounds on 01-14,15-90.
The toluene surrogate recoveries were below EPA CLP QC limits forsamples SB-4-5-1 and SB-4-5-1 MSD. All associated positive resultsand quantitation limits are qualified estimated and flagged "J andUJ11.
Soil samples SB-3-7-1, SB-3-7-2, and SB-3-7-5 required 62.5-folddilutions due to high levels of target compounds. The surrogaterecoveries were not able to be obtained due to these dilutions. Noqualification is applied.
The 2-butanone response factors for initial and continuingcalibrations was below the EPA QC limit of 0.05. The correspondingquantitation limits are rejected.
The blanks contain the common contaminant methylene chloride atlevels less than 5x the CRQL. All associated positive results areless than lOx the blank level; therefore, the quantitation limitsare adjusted to the level of the value reported and are flagged"U". The soil blanks also contain 4-methyl-2-pentanone and 2-hexanone at levels less than the CRQL; however, there were nocorresponding positive sample results for these compounds.
Several compounds had %RSD and %D for initial and continuingcalibrations exceed the 30% and 25% EPA CLP QC limits. Theassociated positive results and quantitation limits are qualifiedestimated "J and UJ".
6R302975
II1
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 9001L127PAGE 3 OF 7
The matrix spike recoveries for toluene 38/37 and chlorobenzene58/53 are below the EPA CLP QC limit of 59% and 60% in sampleSB-4-5-1. The original sample analysis contains both of thesecompounds; therefore, the calculation of the spike recoveries wasprobably affected. Also, for sample SB-1-1-4 MS, thetrichloroethane spike recovery (134%) was above the EPA QC limit of120%* Therefore, a reliable evaluation of the long term precisionand accuracy of the analytical method does not exist. Noqualification is applied on this basis alone.
The 50ng standard was not listed on the Form VI for the initialcalibration on 01-09-90. The Form VI and corresponding Form VII'swere corrected and are submitted with this report. All associatedqualifications reference the corrected forms.
The incorrect received date of 01-11-90 is listed throughout thedata package. The correct received date, according to the chain-of-custody, is 01-10-90. The usability of the data is notaffected.
Sample SB-3-7-5 was missing the spectra/library search for vinylacetate and the Form VIII was missing from samples SB-l-l-4, SB-1-1-4 MS/MSD, SB-l-l-3, and VBLKLVQ015-MB1. The missing pages aresubmitted with this report.
flR302976
II
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 9001L127PAGE 4 OF 7
EVALUATION BY FRACTION
II. Base/Neutral/Acids
x Holding Time___ Extraction Time___ Surrogate Recoveryx Blankx MS/MSD___ GC/MS Tuningx Initial Calibrationx Continuing Calibration___ Compound ID (HSL, TIC)___ Standards___ Spectra Quality___ Chromatography___ Data Completeness
This portion of the case consisted of one water and four soilsamples which were analyzed according to CLP SOW 02/88 (Rev. 05/89)for TCL and client specified semivolatile target compounds on02-01,07,08,09,20,22,23-90.
Samples SB-3-7-1, SB-3-7-2, SB-3-7-5, and SB-4-5*! were re-analyzedoutside the EPA QC holding times because the laboratory stated thatthey were accidentally spiked with the spiking compounds. However,due to the dilutions required (high levels of target compounds) ,all surrogate and spike compounds were diluted out. The two setsof sample results were compared and there was little variationbetween values. Therefore, the original analysis results are to beused as the representative values. No qualification has beenapplied.
The soil laboratory blanks contained di-n-butylphthalate, bis(2-ethylhexyl)phthalate (common contaminants), 1,4-dichlorobenzene,1,2-dichlorobenzene, and 1,2,4-trichlorobenzene at levels less thanthe CRQL. The associated samples did not contain any commoncontaminants; however, there were positive results for the othertarget compounds. All sample results less than 5x the blank levelhave had the quantitation limit adjusted to the value reported andwere flagged "U". All other results greater than 5x the blankcontamination are believed to be true values.
Several compounds had %RSD and %D in the initial and continuingcalibrations exceed the 30% and 25% EPA CLP QC limit. Allassociated guantitation limits are qualified estimated "UJ".
flR302977
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 9001L127PAGE 5 OF 7
The matrix spike/spike duplicate recoveries for sample SB-3-7-1were diluted out. Also, 5 of 22 blank spike recoveries are outsideEPA CLP QC limits. Therefore, this is not a reliable evaluation ofthe long term precision and accuracy of the analytical method.However, no qualification is applied on this basis alone.
The received date of 01-11-90 is incorrect throughout the package.The correct date is 01-10-90 according to the chain-of-custody.The data usability is not affected.
The following nine client specified compounds were library searchedand several were detected in these samples:
AnilineN-nitrosodiphenylamineBenzidine1,2,3-Trichlorobenzene1,3,5-TrichlorobenzenePentachlorobenzenel-chloro-3-nitrobenzene1,2,4,5-tetrachlorobenzene1,2,3,4-tetrachlorobenzene
AR3Q2978
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 9001L127PAGE 6 OF 7
EVALUATION BY FRACTION
III. Pesticides/PCB
___ Holding Time___ Extraction Timex Surrogate Recovery
_JC__ MS/MSD___ Blank___ Linearity Calibration___ DDT/Endrin Degradation___ Analytical Sequence___ DEC Retention Timex Continuing Calibrationx Retention Time Window___ Standards___ Chromatography___HSL Compounds___ Data Completeness
This portion of the case consisted of one water and four soilsamples which were .analyzed for TCL Pesticide/PCB target compoundson 02-08,09-90.
The following samples required dilution due to high levels of non-target compounds:
Sample Dilution Factor
SB-3-7-1, MS/MSD 2/5/5SB-3-7-2 2SB-3-7-5 2SB-4-5-1 10
The surrogate recoveries for sample SB-4-5-1 could not be obtaineddue to interference of non-target compounds. Also, PBLKLE0054 wasnot spiked with the surrogate compound. Since surrogate recoveriesare only advisory QC limits, no qualification is applied on thisbasis alone.
The 4,4*-DDT matrix spike recovery (147%) and the matrix spikeduplicate recovery for gaima-BHC (45%) were outside the EPA QClimits of 134% and 46%. Spike recoveries are also advisory;therefore, no qualification has been applied.
The blank spike duplicate was not spiked with spiking compounds.There is no impact to the data since these compounds were notdetected in the samples.
AR302379
l» QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 9001L127PAGE 7 OF 7
Eleven (11) %D's exceeded the 20% QC limit on the confirmationcolumn; but these compounds were not detected in the samples;therefore, there is no impact on the data.
The retention time for endrin on the confirmation column (02-08-90at 06:47) exceeded the established retention time window. Thiscompound was not detected in the samples; therefore, there is noimpact on the data.
flR302980
GLOSSARY OF DATA QUALIFIERS
CODES RELATING TO IDENTIFICATION
(confidence concerning presence or absence of compounds)
0 = NOT DETECTED, SUBSTANTIALLY ABOVE THE LEVELREPORTED IN LABORATORY OR FIELD BLANKS.
R = UNRELIABLE RESULT. ANALYTE MAY OR MAY NOT BEPRESENT IN THE SAMPLE. SUPPORTING DATANECESSARY TO CONFIRM RESULT.
N = NEGATED COMPOUND WAS CONSIDERED AS NOTPRESENT IN THE SAMPLE.
(NO CODE) » CONFIRMED IDENTIFICATION
CODES RELATING TO QUANTITATION
(can be used for both positive results and sample guantitationlimits):
J = ANALYTE PRESENT. REPORTED VALUE MAY NOT BEACCURATE OR PRECISE.
UJ = THE REPORTED QUANTITATION LIMITS AREQUALIFIED ESTIMATED.
OTHER CODES
NO ANALYTICAL RESULT.
H*-i \c> *-» \n tJ* H0) I O-H r>a X Kto o O • \ It ^I CO «H D> tl H*• 3 (II IICD liW H ^
<w p P 05 1^" -^i ^ o ooo
i w o^« *0 *fn 3 II 10 rHI IIffl IICQ li
•-* ^ _<H P P tfIIw -^ iH in t7> II o
I O -H * II Or^ o o M \ li oI w \o cr> II fn 3 » in! IIffi IIco iir-i HD >o<w P P K
I!rH r> »H in en II oI O -H • || Or- o o fs \ II oI 09 \D CP It <n 3 It int IICQ IICO Ii
H b ^J ^<w p p P « P„ Itn CM J-j H J II \oI O 0) \ II•H O -P tT III 1C D II•-f ^ III IIm i!CO II
-t hi _ ^<w P P o; pii^•pH^^iJl! r-vDI O 0) \ ii HH O -P CT HI (0 S IIH S III IICQ IICO IIII ................D S X • 03 IIH &H -M fo -p IIK U "H ||
4J 4^ Q C IIW (0 p H
II ......... c ........ 0 •• • * «Jii ......... o> ........ c • • • • ao11 ......... oj ... (0 0)if .... 0 .. o a> oItIt . . . »-HII • • . • JqII • • O - ONO • *O • r-iii c o -H a) :
C I! fl C M C OO (I J (0 0 (0-H ii *» /: H jc a)
fl) O (0 0•O 3 & *-4-H .a) a) a
OQ
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<u oO H
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fiR302989
1A CLIENT SAMPLE NO.VOLATILE OHGAMICS ANALYSIS SHEET ________________
|SB-3-7-5HIM: Rov F. ge«ton. Inc. Work Orders 2267-09-02-0000 j______
Client: STANDARD CHLORINE______
Matrix: SOIL Lab Sample ID: 9001L127-005
Sample wt/vol: 4.00 (g/fflL) g_ Lab File IDs Y011506
Level: (low/mod) *SP_ Date Received: 01/11/90
% Moieture: not dec. ___i Date Analyzed: 01/15/90
Coluon: (pack/cap) £ACK Dilution Factor: 62.5
CONCENTRATION UNITS:CA5 NO. COMPOUND (ug/L or ug/Kg) UQ/KC
74-87.3———————Chloromethane___________74-83-9———————Bromomethane____________7S-01-4——————Vinyl Chloride__________7S-00-3——————Chloroethane___________7S-09-2——————Methylene Chloride______67-64-1———————Acetone________________75-15-0——————Carbon Disulfide________75-35-4———————1,1-Dichloroethene______75-34-3———————1,1-Dichloroethane_______540-S9-0——————1,2-Dichloroethene (total)_67-66-3———————Chloroform_____________107-06-2——————l,2-0ichloroethane__78-93-3———————2-Butanone_________71-55-6———————l,lpl-Trichloroethane_S6-23-5——————Carbon Tetrachloride__108-05-4——————Vinyl Acetate_______75-27-4———————Broffiodichloromethane____78-87-5———————1,2-Dichloropropane_____10061-01-5————cia-lf3-Dichloropropene__79-01-6———————Trichloroethene_________124-48-1———•——Dibromochloromethane____79-00-5——————1,1,2-Trichloroethane___71-43-2 ———————Benzene___ ' ' • '___'10061-02-6————Tran»-l,3-Dichloropropene_75-25-2———————Bronoform_____________108-10-1——————4-Kethyl-2-pentanone____591-78-6——————2-Hexanone____________127-18-4——————Tetrachloroethene_______79-34-5———————1,1,2,2-Tetrachloroethaue_108-88-3——————Toluene_______________108-90-7——————Chlorobenzene___________100-41-4——————Ethylbenzene___________100-42-5——————Styrene_______________1330-20-7—————Xylene (total)
66000 |U66000 JU66000 JU66000 j D56000 JB66000 |U33000 |U33000 |U33000 |U33000 |U33000 JU33000 |U66000 |U33000 |U33000 JU66000 |U33000 |033000 |D33000 |U33000 |U33000 JU33000 |U33000 |U33000 |U33000 |U66000 |U66000 |D33000 |D33000 JU33000 |0530000 j33000 |U33000 |U33000 |U
FORK 1 V-l 12/88 Rev.
fiR302990
6AVOLATILE ORGANICS INTITIAL CALIBRATION DATA
Lab Hame: Rov F. Weston, Inc. Contract: $3L*)~Oe!~G3.'~
Ca»* NO.J 3tg gu?* r Chfo^tH€ RFW Lot:
Instrument IDs 5100Y *_... Calibration Date(s): 01/09/90 01/09/90
Matrix: (soil/water) Level: (low/mad) MED Column: (pack/cap) PACK
Kin RRF for SPCC(I) » 0*300 {0.250 for Broooform) Max %RSD for CCC(*) « 30.0%
ILAB FILE ID: RRKO - yoi0904IRRFIOO- Y0io9os RRFISO- YOiogoe1I 1 I| COMPOUND | RRF 20 |RRF50
| Chloromethane * 1.341 | 0.896| Brocnomethane | 1.531 | 1.316|Vinvl Chloride * 1.595 | 1.486|Chloroethane 1 0.893 | 0.855|Hethylene Chloride | 2.472 | 1.536| Acetone 1 0.759 f 0.853(Carbon Dieulfide | 4.116 | 3.927|l.l-Dichloroethene * 1.340 | 1.238|l,l-Dichloroethane * 2.894 | 2.694|l,2-Dichloroethene (total) ___ | 2.753 | 2.4371 Chloroform * 2.637 | 2.463|1.2-Dichloroethane | 1.852 | 1.687|2-Butanone | 0.013 | .0050|l.l.l-Trichloroethane | 0.606 | O.S77(Carbon Tetrachloride _, „,, ., | 0.527 | O.B13|vinvl Acetate 1 | 0.084(Bromodichloromethane _| 0.675 | 0.626(1.2-Dichloroorooane * 0.497 | 0.464|ci«-lf 3-Dichloropropene | 0.667 | 0.620|Trichloroethene 1 0.515 | 0.511|Dibromochloromethane | 0.640 | 0.623|l,l,2-Trichloroethane | 0.352 | 0.3141 Benzene | 1.080 | 0.994| Trane-1, 3-Dichloropropene ___ | 0. 509 | 0 . 445iBrocooform * 0.456 j 0.472|4-Methyl-2-pentanon« | 0.4B5 | 0.455|2-Hexanone ! 0.328 | 0.311(Tetrachloroethene | 0.620 | 0.57911,1,2,2-Tetrachloroethane ___ * 0.577 | 0.531[Toluene * 0.729 j 0.661]Chlorobenzene * 1.038 | 0.945|Ethylbenzene * 0.472 | 0.434(Styrene | 0.880 | 0.836|Xylene ftotall , 1 0.981 | 0.917t(Toluene-d8 | 1.176 | 1.097| Brotnof luorobenzene | 0.885 | 0.830|l,2-Dichloroethane-d4 | 1.742 | 1.6421 ! 1
RRP50 " Y010903RRF200- Y010907
RRF100
0.6911.2941.4590.7941.4210.757
73.7761.1342.65S2.1122.2831.632.00700.5680.5180.0830.6690.4860.6500.4960.6420.3041.0290.4710.4860.4370.3000.5700.5140.6620.9190*4290.8390.927
1.1280.8631.581
RRF150
0.5211.2671.4190.8021.3840.8823.6441.226'2.6122.0922.3941.781.00800.5600.5430.0950.7140.5180.6980.5140.6970.3271.0910.5220.5570.5140.3530.6100.5780.7300.9870.4660.9401.057
1.2210.9721.736
RRT200
0.3041.3401.5140.8521.3340.8153.7361.1542.6922.2512.3591.635.00700.7030.5610.0690.6940.5070.6810.5100.6870.3211.0530.5110.5260.4730.3140.5690.5350.6770.9270.4400.8851.035
1.0820.8451.504
RRF
0.7511.3501.4950.8391.6390.8133.8401.2182.7102.3292.4271.7170.0080.6030.5320.0700.6760.4940.6630.5090.6580.3241.0490.4920.5000.4730.3210.5900.547•0.6920.9630.4480.8760.983
1.1410.8791.641
% 1RSD |
, ——— .|52.717.8J4.4*4.9|29. OJ6.9|4.8|6.7*4. Of11.815.5*S.6|37. 5|9.7|3.7|2S.9|4-9|4.2*4.5|1.5|4.9)5.613.7|6.618.2*6.2|6.3|4.0|5.3*5.1*5.1*4.4*4.8)6.4|
____|5.0|6.4J6.2|
1FORM VI VOA 01/89 Rev.
ftR30299l
•
*
7AVOLATILE COKTINUING CALIBRATION CHECK
//?•Nam*: Rov F» tfaaton. Inc ' Contract:
Mo.t .S anfifffH/ fJ*l*tone RFW Lot:
Instrument ID* S100Y Calibration Data: 01/15/90 Time: 0856
tab Pile ID: y011SQ2 Init. Calib. Date(»): 01/09/90 01/09/90
Matrix: (soil/water) Level:(low/med) ggD Column* (pack/cap) PACK
Kin RRF50 for SPCC(t) « 0.300 (0.250 for Bromoform Max %D for CCC(*) » 25.0%
1j COMPOUND
| chloromathane| Bromomethana1 Vinyl Chloride| Chloroethane _ ,„„ ,[Methylene Chloride[Acetone| Carbon Diaulfide ,,_„,_, ._,I 1 , 1-Dichloroathene ,1 1 . 1-Dichloroathana ,„ ,_ ,„. ,|l,2-Dichloroath*na (total)| Chloroform| l,2-Dichloro»than» mm i m m m| 2-Butanona[1,1, 1-Tr ichloroethana| Carbon Tatrachloride(Vinyl Acatata! Brcmodichloromethanc| 1.2-Dichloropropan«[ cii-1 , 3-Dichloropropene| Trichloroathana _,_.„.„| Dibromochloromathana| l,1.2-Trichloro»than«[ B«nz«no| Trani-1 , 3-Dichloropropana-| Bromoform] 4-Hathyl-2-pentanone| 2*Eaxanona| Tatrachloroathana1 1,1,2,2-Tatnchloroethan*| Tolucn*| Chlorobenzana| Ethylb«nzen»| Styrane|Xvlena (total)1| Tolu«ne-d8| Bromof luorobenzene| l,2-Dichloro«thane-d41
| RRF
* 0.751| 1.350* 1.495| O.S39| 1.639! 0.613| 3.840* 1.218* 2.710| 2.329* 2.427| 1.717| 0.0081 0.6031 0.532| 0.0701 0.676* 0.494| 0.663| 0.5091 0.658| 0.3241 1.049
_ 1 0.492* 0.500| 0.473
_ 1 '0.321| 0.590* 0.547* 0.692
._....§ 0.963* 0.448| 0.876| 0.983
| 1.141| 0.879I 1.6411
RRF050
0.6801.5281.6880.9841.7980.8444.4321.4113.0703.0922.9931.813.00400.5370.4740.0720.6480.4890.6470.5160.5940.3191.0910.4660.4460.4280.2850.6060.5390.7321.0020.4670.9221.060
1.1870.8921.735
|%D |
9.5 #/-13.2 |-12.9 * /-17.3 |-9.7 I-3.8 |-15.4 |-15.8 * S-13.3 */-32.8 |-23.3 * /-5.6 |50.0 |10.9 |10.9 1-2.9 |4.1 |1.0 */2.4 |-1.4 |9.7 |1.5 |
-4.0 15.3 |10.8 #/9.5 |11.2 |-2.7 |1.5 */
-5.8 *S-4.0 #/-4.2 */-5.3 |-7.8 |
——- ——— 1-4.0 |-1.5 I-5.7 |
1FORM VII VOA 5/B8 Rev.
RR302992
7AVOLATILE CONTINUING CALIBRATION CHECK
Lab Name: Rov y. Waaton, Inc. Contract i
Caa« No.: SbnJad cJ*/0HHe RFW Lot:
Instrument 10: 5100Y * Calibration Dates 01/14/90 Time: 1242
Lab Fil« ID: Y011402 Init. Calib. Dat»(«): 01/09/90 01/09/90
Matrix: (soil/water) Levels (low/med) %j£L Column: (pack/cap) PACK
Kin RRF50 for SPCC(f) * 0.300 (0.250 for Bromoform Max %D for CCC{*> * 25.0%
COMPOUND | RR? (RRP050
| Chloromethane| Bromome thane(Vinvl Chloride| Chloroethane(Methvlene Chloride(Acetone(Carbon Disulfide1 1 . 1-Dichloroethene( 1. 1-D ichloroethane , ,|l,2-Dichloroethene (total)| Chloroform| 1, 2-D ichloroethane(2-Butanone(1,1. 1-Tr ichloroethane| Carbon Tetrachloride| Vinvl AcetatefBromodichloromethane| 1 . 2-Dichloropropane| cia-1 , 3-Dichloropropene| Trichloroethene| Dibromochloroinethane( 1 . 1 . 2-Tr ichloroethane| Benzene| Trans-1, 3-Dichloropropene| Bromof orm| 4-Methyl-2-pentanone1 2*Hexanone| Tetrachloroethene| 1,1,2,2-Tetrachloroethane| Toluene| Chlorobenzene(Bthylbenzene| Stvrene|lvlene f total)
| Toluene-dS| Bromof luorobenzene| l,2-Dichloroethane-d41
# 0.7511 1.350* 1.495| 0.839f 1.639| 0.8131 3.840* 1.218* 2.7101 2.329* 2.4271 1.7171 0.0081 0.6031 0.5321 0.0701 0.676* 0.494| 0.6631 0.5091 0.658| 0.3241 1.049| 0.492I 0.500| 0.473| 0.321| 0.590* 0.547* 0.692# 0,963* 0.448| 0.876F 0.983
1 1.1411 0.8791 1.6411
0.3051.4241.3040.9901.8870.8594.1241.3163.0932.8482.7801.905.00700.6180.5360.0890.7340.5570.7070.4860.6080.3261.1580.5370.4280.4780.3360.5810.5540.7471.0050.4730.9331.062
1.2110.9531.763
».»«.«*59.4 1-5.5 |12.8 *-18.0 |-15.1 |-5.7 |-7.4 |-8.0 --14.1 i-22.3 |-14.5 *-10.912.5-2.5-0.8-27.1-8.6-12.8 *-6.64.57.6-0.6-10.4-9.114.4 J-1.1-4.71.5-1.3 1-7.9 *-4.4 |-5.6-6.5-8.0
-6,1-8.4-7.4
%D
/
/
FORM VII VOA 5/88 Rev.
AR3Q2993
Irii
8AVOLATILE INTERNAL STANDARD AREA SUMMARY
Lab Name i RQV F« Weston, Inc.*. - Contract: 2267-09-02-0000
Case Ho.: STANDARD CHLORINE_____ RFW Lot: 9001L127
Lab File ID (Standard) x "Q011502 Date Analyzed: 01/15/90
Instrument ID: 10SOQ Time Analyzed2 1125
Matrix: (soil/water) EATER Level:(low/med) I£W Columns (pack/cap) PACK
0102030405
12 BOOR STD
UPPER LIMIT
LOWER LIMIT
CLIENT SAMPLENO.
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f Column used to flag internal standard area values with an asterisk
page 1 of 1 FORM VIII VOA 5/88 Rev.
AR30299U
STANDARDCASE 89X1L554
This quality assurance review is based upon a review of the datagenerated from two water and three soil samples collected on11-17-89 and analyzed by Roy F. Weston Lionville AnalyticalLaboratory for TCL Volatile, Semivolatile, and Pesticide/PCB targetcompounds.
The reported analytical results are presented as a summary of thedata in Section II. All of the analytical data were examined todetermine the usability of the analytical results and also todetermine contractual compliance relative to the analyticalrequirements and deliverables specified in EPA's ContractLaboratory Program (CLP) protocol. Qualifier codes have beenassigned next to the results so that the data user can quicklyassess the qualitative and/or quantitative reliability of anyresults.
Details of this quality assurance review are presented in thenarrative section of this report under each fraction. This reportwas prepared to provide a critical review of the laboratoryanalyses and reported analytical results.
AR302995
Irii
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L554PAGE 2 OF 7
BVALUATIOH BY FRACTION
I. Volatiles
Holding TimeSurrogate RecoveryMS/MSDBlankGC/MS TuningInitial CalibrationContinuing CalibrationCompound ID (HSL, TIC)
___ Standards___ Spectra Quality___ Chromatographyx Data Completeness
This portion of the case consisted of two water and three soilsamples which were analyzed according to CLP SOW 02/88 (Rev. 05/89)for TCL Volatile target compounds on 11-24,27,28,29,30-89.
Sample SP-1-2-1 matrix spike/spike duplicate were analyzed two andone day outside the holding time, respectively, Al 1 positiveresults and guantitation limits for these QC samples are consideredestimated.
The following surrogate recoveries are slightly below the EPA CLPQC limits:
Sample ID Surrogates
SP-1-2-4 Toluene, BromofluorobenzeneSP-1-2-4, MS Toluene, BromofluorobenzeneSP-l-2-4, MSD BromofluorobenzeneSP-1-2-3 Toluene, BromofluorobenzeneSP-1-2-3-DL Toluene, 1,2-Dichloroethane
All associated positive results and guantitation limits for thesesamples are considered estimated and are flagged "J and UJHrespectively, in the data summary.
2-Butanone had response factors less than 0.05 in"the initial andcontinuing calibrations. The reported quantitation limits for allsamples have been rejected and flagged "R" in the data summary.
SR302996
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L554PAGE 3 OF 7
The blanks contain common contaminants methylene chloride andacetone at levels less than 5x the CRQL. All associated positiveresults that are less than lOx the blank level, have theguantitation limits adjusted to the reported value and are flagged"U" in the data summary- The methylene chloride in sample SP-1-2-3-DL was above lOx the blank level; therefore, this is considereda true value. Blank (89LVQ210) also contained carbon disulfide ata level less than the CRQL. However, there were no associatedpositive results for this compound.
Several compounds had %D in the continuing calibrations exceed the25% EPA CLP QC limits. All associated quantitation limits areconsidered estimated and are flagged "UJ".
Most water and soil matrix spike recoveries are outside the EPA CLPQC limits as well as the %RPD. The soil spike recoveries wereconsidered diluted out due to the medium level analyses. On thisbasis alone, no qualification is applied; however, the recoveriesare not considered a good judge of the long term precision andaccuracy of the analytical method.
Sample SP-1-2-3 required a two-fold dilution due to a high level ofmethylene chloride. The diluted result, for this compound only,should be used as the true value. All other compound results comefrom, and are qualified based on, the original analysis.
All soil samples required medium level analyses due to high levelsof target compounds. The surrogate recoveries for SP-1-2-1, MS,MSD were diluted out.
Sample SP-1-2-3DL was missing the spectra for methylene chloridefrom the original data package. The spectra is submitted with thisreport.
Dichlorobehzene compounds were detected as Tentatively IdentifiedCompounds (TIC's) in several samples.
AR302997
I
I
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L554PAGE 4 OF 7
EVALUATION BY FRACTION
II. Base/Heutral/Acids
Holding TimeExtraction TimeSurrogate Recovery • 'BlankKS/MSDGC/MS TuningInitial CalibrationContinuing CalibrationCompound ID (HSL, TIC)StandardsSpectra Quality
___ Chromatography___ Data Completeness
This portion of the case consisted of one water sample and threesoil samples which were analyzed according to CLP SOW 02/88 (Rev.05/89) for TCL and client specified Semivolatile target compoundson 11-29,30-89 and 12-28,29-89.
The soil samples required high level dilutions (5550-fold) due tothe level of target compound 1,4-dichlorobenzene. In the case ofsample SD-1-3-5, it was originally analyzed at a 1110-fold dilutionand then re-analyzed at 5550-fold so that the 1,4-dichlorobenzenevalue would be within the calibration range. It is the dilutedresult that is used for this compound, all other results are fromthe original analysis. Also, due to these large level dilutions,the surrogate and matrix spike recoveries could not be obtained.
Several compounds had %RSD and %D for initial and continuingcalibrations exceed the 30 and 25% EPA CLP QC limits. Allassociated guantitation limits are qualified estimated and flaggedKUJ" in the data summary.
The laboratory blanks contain several target compounds at levelsless than the CRQL. In the case of the water blank, the associatedsample contains the same compounds di-n-butylphthalate and bis(2-ethylhexyljphthalate at levels less than 10X the blankcontamination. Therefore, the samples quantitation limits forthese .compounds are adjusted to the value reported and are flaggedWU" in the data summary. The soil blank also contained targetcompounds at levels less than the CRQL, but the associated samplesdid not contain the same compounds.
AR3G2998
I QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L554PAGE 5 OF 7
! F i v e of 22 blank spike recoveries exceeded the EPA CLP QC limits.All %RPD met criteria. No qualification is applied on this basisalone, since spike samples are used to judge the long termprecision and accuracy of the analytical method.
The following nine client specified compounds were library searchedand were not detected in any of these samples: aniline, n-nitroso-dimethylamine, benzidine, 1,2,3-trichlorobenzene, 1,3,5-trichloro-benzene , 1,2,4, 5-tetrachlorobenzene, 1,2,3, 4-tetrachlorobenzene,pentachlorobenzene and l-chloro-3-nitrobenzene.
flR302999
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L554PAGE 6 OF 7
XVM.0AMON BY FRACTION
III. Pesticides/PCB
___ Holding Time___ Extraction Timex Surrogate Recovery
_J£_ MS/MSD___ Blankx Linearity Calibration___ DDT/Endrin Degradation___ Analytical Sequence___ DBC Retention Timex Continuing Calibrationx Retention Time Window___ Standards___ Chromatography___ HSL Compounds___ Data Completeness
This portion of the case consisted of one water and two soilsamples which were analyzed for TCL Pesticide/PCB target compoundson 11-30-89, and 12-01,14-89.
The soil samples required 10-fold dilutions due to high levels ofcompounds. No other pesticide compounds were detected in thesesamples except for several arochlors. The surrogate recoveriescould not be obtained for these samples due to compoundinterference.
The surrogate recovery for PBLKLE1165-MB1 (19%) was below the EPACLP advisory QC limit of 24%. Since surrogate recoveries haveadvisory limits, no qualification is applied on this basis alone.
The matrix spike/spike duplicate recoveries for endrin (1/36%) andfor gamma-BHC (I/I) in sample SP-1-3-S were outside the QC limits.The original sample and QC samples contain higher levels of non-target compounds that probably interfered with the matrix spikerecoveries. These compounds were not detected in the samples;therefore, no qualification is applied.
Ten of 12 blank spike recoveries were below EPA CLP QC limits.There is no impact on the data since these compounds were notdetected in the samples.
fiR303000
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L554PAGE 7 OF 7
The %RSD for aldrin (22.3%) is outside the 10% QC limit. The casenarrative stated that the concentration in EVAL C is outside thelinear range on the primary column using LIMS calculations.However, the data is within the linear range, of the Hewlett-Packard(H-P) integrator. The reported guantitation limits for aldrin inthe soil sample are qualified estimated "UJ".
The %D on the primary column analyzed on 12-13,14-89 for dieldrin,DOT, heptachlor epoxide (IND A 12-13-89 at 09:52), heptachlorepoxide, dieldrin (IND A 12-14-89 at 03:20), endosulfan sulfate(IND B 12-14-89 at 19:22), and delta-BHC endosulfan sulfate (IND B12-14-89 at 22:43) exceeded the 15% requirement limits. However,none of these compounds were detected in the samples; therefore,there is no impact to the data.
Several %D also exceeded the 20% QC limit on the confirmationcolumn, but those target compounds were not detected in thesamples. Therefore, there is no impact to the data.
The retention time criteria on both columns were outside thes established retention time window for several compounds analyzed— prior to the samples: primary column - 4,4-DDT (12-14-89 at 03:20),
4,4-DDD, endosulfan sulfate (12-14-89 at 19:22) and confirmationcolumn - endosulfan sulfate, endrin ketone (12-14-89 at 09:27).These compounds were not detected in the samples; therefore, thereis no impact to the data.
Up to eleven other retention time criteria on both columns wereoutside QC limits. The data is not affected since thesecalibrations were analyzed at the end of the sample analyses.
AR303QO
INFORMATION REGARDING DATA
All data were reviewed according to EPA CLP Functional Guidelinesfor Evaluating Organic Analyses. All data have been validated withregard to usability.
If you have any questions or comments on this data review, pleasecall Zohreh Hamid at (215)524-7360.
1. Glossary of Data Qualifier Codes.
2. Data Summary. This includes:
a) All positive results for the target analyteswith the qualifier codes, if applicable; and
b) All unusable detection limits (qualified "R") .
3. Support Documentation includes details to support thestatements in this reports.
flR303002
IGLOSSARY OF DATA QUALIFIERS
CODES RELATING TO IDENTIFICATION
(confidence concerning presence or absence of compounds)
0 » NOT DETECTED, SUBSTANTIALLY ABOVE THE LEVELREPORTED IN LABORATORY OR FIELD BLANKS.
R « UNRELIABLE RESULT. ANALYTE MAY OR MAY NOT BEPRESENT IN THE SAMPLE, SUPPORTING DATANECESSARY TO CONFIRM RESULT.
N » NEGATED COMPOUND WAS CONSIDERED AS NOTPRESENT IN THE SAMPLE.
(NO CODE) CONFIRMED IDENTIFICATION
COPES RELATING TO OUANTITATION
(can be used for both positive results and sample quantitationlimits):
J « ANALYTE PRESENT. REPORTED VALUE MAY NOT BEACCURATE OR PRECISE.
0J - THE REPORTED QUANTITATION LIMITS AREQUALIFIED ESTIMATED.
OTHER CODES
NO ANALYTICAL RESULT..
AR3030-OU
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flR3030i2
STANDARD CHLORINECASE 8911L574
This quality assurance review is based upon a review of the datagenerated from one aqueous and two soil samples collected on11-20-89 and analyzed by Roy F. Weston Lionville AnalyticalLaboratory for TCL Volatile, Semivolatile, and Pest/PCB targetcompounds.
The reported analytical results are presented as a summary of thedata in Section II. All of the analytical data were examined todetermine the usability of the analytical results and also todetermine contractual compliance relative to the analyticalrequirements and deliverables specified in EPA's ContractLaboratory Program (CLP) protocol. Qualifier codes have beenassigned next to the results so that the data user can quicklyassess the qualitative and/or quantitative reliability of anyresults.
Details of this quality assurance review are presented in thenarrative section of this report under each fraction. This reportwas prepared to provide a critical review of the laboratoryanalyses and reported analytical results.
AR3030U
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L574PAGE 2 OF 7
EVALUATION BY FRACTION
I. Volatiles
Holding TimeSurrogate RecoveryMS/MSDBlankGC/MS TuningInitial CalibrationContinuing CalibrationCompound ID (HSL, TIC)StandardsSpectra QualityChromatographyData Completeness
This portion of the case consisted of two water and two soilsamples which were analyzed according to CLP SOW 02/88 (Rev. 05/89)for TCL Volatile target compounds on 11-24,27-89.
2-Butanone and 4-methyl-2-pentanone had response factors less thanthe 0.05 EPA CLP QC limit in the soil initial and continuingcalibrations. The quantitation limits for all soil samples havebeen rejected and flagged "R" in the data summary.
The samples below had the following surrogate recoveries andinternal standards outside the QC limits:
Surrogates Internal StandardsSample ID r , (Exceeded EPA QC Limits) Below Control Limit
SR-4-1-1 Toluene, 1,2-Dichloroethane NoneSR-4-1-1, MS Toluene, 1,2-Dichloroethane All StandardsSR-4-1-1, MSD 1,2-Dichloroethane All StandardsSR-4-1-2 Toluene, 1,2-Dichloroethane Chlorobenzene-d5SR-4-1-2 RE Toluene, 1,2-Dichloroethane All Standards
The surrogate recovery and internal standard outliers seem to beassociated with the soil matrix. Results may be biased high;therefore, the positive results and guantitation limits for allsoil sample analyses are considered estimated and are flagged "Jand UJ".
AR3G3015
I! QA ORGANIC DATA REVIEW
STANDARD CHLORINECASE 8911L574PAGE 3 OF 7
Several compounds had %RSD and %D for water analyses in the initialand continuing calibrations exceed the 30% and 25% EPA CLP QClimits. All associated quantitation limits are consideredestimated and are flagged "UJ".
The soil blanks contain common contaminant methylene chloride atlevels less than 3x the CRQL. All associated positive results arebelow lOx the level in the blank; therefore, the quantitationlimits are adjusted to the reported value and are flagged with a"U" in the data summary.
Two of 10 soil matrix spike recoveries and all % RPD were below EPACLP QC limits. No qualification is applied on this basis alone;however, this set of QC samples should not be used to judge thelong term precision and accuracy of the analytical method.
The results for % relative abundance for m/e = 176 on tunesanalyzed on 11-14-89 (HP-MSDX) and 11-27-89 (HP-MSDX) were notcompletely calculated. The corrected Form V's are re-submitted.
flR3030i6
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L574PAGE 4 OF 7
EVALUATION BY FRACTION
II. Base/Neutral/Acids
___Holding Time___ Extraction Timex Surrogate Recoveryx Blankx MS/MSD___ GC/MS Tuningx Initial Calibrationx Continuing Calibration___ Compound ID (HSL, TIC)___ Standards___ Spectra Quality___ Chromatographyx Data Completeness
This portion of the case consisted of two soil samples and onewater sample which were analyzed according to CLP SOW 02/88 (Rev.05/89) for TCL and client specified semivolatile target compoundson 12-20,28,29*89.
The 2-fluorobiphenyl surrogate recovery for SBLKLE1176-MB1 BS andSBLKLE1176-MB1 BSD were below the EPA CLP QC limits. Since the BSDis the re-analysis of the BS, both sets of data's positive resultsand guantitation limits are considered estimated.
Several compounds had %RSD and %D in the initial and continuingcalibrations exceed the 30 and 25% EPA CLP QC limits. Allassociated guantitation limits are considered estimated and areflagged "UJ" in the data summary.
The laboratory blanks contain common contaminant di-n-butylphthalate at a level less than 5X the CRQL. Blank 89LE1178also contains 1,4-dichlorobenzene at a level less than the CRQL.The soil samples contain 1,4-dichlorobenzene at levels greater than5X the blank contamination; therefore these results are consideredtrue values and no qualifier codes are applied. In the case of di-n-butylphthalate, the samples have levels less than 10X the blanklevel. Therefore, the guantitation limits of these samples areadjusted to the reported value and are flagged "U" in the datasummary.
The matrix spike recovery for 1,4-dichlorobenzene exceeds the EPACLP QC limit. The original sample and its associated QC sampleshad high levels of this compound; thus affecting the spike recoveryresults. No qualification is applied.
5R3030I7
Ir QA ORGANIC DATA REVIEW
STANDARD CHLORINECASE 8911L574PAGE 5 OF 7
Five of 22 blank spike recoveries are below the EPA CLP QC limits.No qualification is applied on this basis alone, since spikerecoveries are only used judge the long term precision and accuracyof the analytical method.
The di-n-butylphthalate spectra was missing from blank (89LE1176)in the original data package. The 'spectra has been submitted withthis report.
The following nine client specified compounds were library searchedand sample SR-4-1-1 contained 1,2,3,4-tetrachlorobenzene at a levelless than the CRQL: aniline, n-nitrosodiphenylamine, benzidine,1,2,3-trichlorobenzene, 1,3,5-trichlorobenzene, 1,2,4,5-tetrachlorobenzene, 1,2,3,4-tetrachlorobenzene, pentachlorobenzeneand l-chloro-3-nitrobenzene.
BR303018
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L574PAGE 6 OF 7
EVALUATION BY FRACTION
III. Pesticides/PCB
___ Holding Time___ Extraction Time___ Surrogate Recovery___ MS/MSDx Blank
__x_--Mnearity Calibration___ DDT/Endrin Degradation___ Analytical Sequence___ DEC Retention Timex Continuing Calibrationx Retention Time Window___ Standards___ Chromatography___ HSL Compoundsx Data Completeness
The soil blank (89LE1178-MB2) contains DDD at the level 30 ug/kg.This compound was detected in soil sample SR-4-1-2 at the levelless than the CRQL. Therefore, the reported result in this sampleis qualified "U" and should be considered not present in thesample.
The spike recovery for aldrin (35%) in the blank spike, dieldrin(134%), and endrin (126%) in the blank spike duplicate were outsidethe QC limits. The case narrative stated that the negative peaksin gas chromatogram caused a high integration for dieldrin andendrin in blank spike duplicate sample. There is no impact to thedata since these compounds were not detected in the samples.
All relative percent difference are exceeded in water blank sampleThe precision of the reported results are questionable; however,the target compounds were not detected in the samples.
The %RSD for aldrin (22.3%) is outside the 10% QC limit. The casenarrative stated that the concentration of aldrin in EVAL C isoutside the linear range on the primary column using LIMScalculations. However, the data is within the linear range ofHewlett Packard (H-P) integrator. The reported data for aldrin inthe soil samples are qualified estimated.
SR303019
II
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L574PAGE 7 OF 7
The %D on the primary column analyzed on 12-13,14-89 for dieldrin,DDT (IND A 12-13-89 at 9:52) and heptachlor epoxide, dieldrin (INDA 12-14-89 at 3:30) exceeded the 15% requirement limits in soilsample analysis.
The calibration fraction for the above compounds were exceeded inthe continuing calibration; therefore, the reported results for DDTin sample SR-4-1-2 could be biased high. Other compounds were notdetected in the samples; therefore, there is no impact to the data.
Also, %D for up to six compounds exceeded the 15% requirement forthe water sample analysis. The response factors were increasedduring the continuing calibration; however, none of the compoundswere detected in the samples. Therefore, there is no impact to thedata
DDT was quantified in the water sample; however, the retention time(of this compound was outside the established retention time window.
The retention time for this compound exceeded the primary andconfirmation analysis performed after the water sample analysis;therefore the reported result for DDT in the water sample qualifiedas estimated. Other compounds had retention time outside theretention time window; however, there is no impact to the dataspike. These compounds were not quantified in the samples.
The retention time criteria for endosulfan sulfate and endrinketone o'n the confirmation analysis performed on 12-14-89 at 9:27exceeded the retention time window. The reported data is notaffected since this calibration was analyzed at the end of thesample analysis. . — -
The guant results were inadvertently listed as "N" on Form IX forprimary column analysis performed on 12-12,13,14-89. These formswere corrected and re-submitted.
A~R303020
INFORMATION REGARDING DATA . . . , . _
All data were reviewed according to EPA CLP Functional Guidelinesfor Evaluating Organic Analyses. All data have been validated withregard to usability.
If you have any questions or comments on this data review, pleasecall Zohreh Hamid at (215)524-7360.
ATTACHMENTS
1. Glossary of Data Qualifier Codes.
2. Data Summary. This includes:
a) All positive results for the target analyteswith the qualifier codes, if applicable; and
b) All unusable detection limits (qualified "R") .
3. Support Documentation includes details to support thestatements in this reports.
GLOSSARY OF DATA QUALIFIERS
CODES RELATING TO IDENTIFICATION
(confidence concerning presence or absence of compounds)
0 = NOT DETECTED, SUBSTANTIALLY ABOVE THE LEVELREPORTED IN LABORATORY OR FIELD BLANKS.
R = UNRELIABLE RESULT. ANALYTE MAY OR MAY NOT BEPRESENT IN THE SAMPLE. SUPPORTING DATANECESSARY TO CONFIRM RESULT.
N = NEGATED COMPOUND WAS CONSIDERED AS NOTPRESENT IN THE SAMPLE.
(NO CODE) = CONFIRMED IDENTIFICATION
CODES RELATING TO OPANTITATION .........
(can be used for both positive results and sample guantitationlimits):
J = --ANALYTE PRESENT. REPORTED VALUE MAY NOT BEACCURATE OR PRECISE.
UJ = THE REPORTED QUANTITATION LIMITS AREQUALIFIED ESTIMATED.
OTHER CODES
NO ANALYTICAL RESULT.
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5AVOLATILE ORGANIC "GC/HS TUNING AND MASSCALIBRATION - ®ROMOFL0OROBENZBNE (BFB)
Lab Name: RQV F» Weaton, Inc» . Contract: 2267-09-02-0000
Case No.: STANDARD CTO3KXNE_____ T
Lab File ID; AXBS01 BFB Injection Date: 1 /14/69
Instrument IDs HP-H5D X BFB Injection Times 719
Matrixi (soil/water) SOIL Level:(low/med) LOW "olumn: (pack/cap) CAP
m/e««»50759596173174175176177
ION ABUNDANCE CRITERIA
15.0 - 40.0% of mass 9530.0 - €0.0% of mass 95Base peak, 100% relative abundance5.0 - 9.0% of mass 95Less than 2.0% of mass 174Greater than 50.0% of mass 955.0 - 9.0% of mass 174Greater than 95.0% but less than 101.0% of mass 174S.O - 9.0% of mass 176
% RELATIVEABUNDANCE
18.950.1
100.06.70.0( 0.
77.3S.5( 7.77. 4( «?.*?
5.7( 7.
0)1
2)1u4)2
1-Value is % mass 174 2-Value is % mass 176
THIS TUNE APPLIES TO THE FOLLOWING SAMPLES, MS, MSD, BLANKS, AND STANDARDS:
02
06 |07 |08109)101HI12|13 |14115116117118119120|
CLIENT | LABSAMPLE NO. j SAMPLE ID
VSTD20 1 VSTD20VSTD50 " | VSTD50VSTD100 1 VSTD100VSTD150 | VSTD150VSTD200 | VSTD200
111111111i
11111
LABPILE ID
AX.BE02AXBE03AXBE04AXBE05AXBE06
DATEANALYZED
11/14/8911/14/8911/14/8911/14/8911/14/89
TIMEANALYZED
08170849092009521024
page 1 of 1 FORM V VOA 1/87 Rev.
AR303032
VOLATILE ORGANIC GC/MS TUNING AND MASSCALIBRATION - BROMOFLUOROBENZENE (BFB)
*ab Name: Roy F. West on f Inc. Contract: 2267-09-02-0000
:ase No.: STANDARD CHLORINE
-ab File ID: AXBR01
Cnstrument ID: HP-MSD X
iatrix : ( soil/water ) SOIL Level : ( low/med )
,1
m/e | ION ABUNDANCE CRITERIA
50 f 15.0 * 40.0% of mass 9575 | 30.0 - 60.0% of mass 9595 | Base peak, 100% relative abundance96 | 5.0 - 9.0% of mass 95173 | Less than 2.0% of mass 174174 | Greater than 50.0% of mass 95175 f 5.0 - 9.0% of mass 174
O *><£0
BFB Injection Date: 11/27/89
BFB Injection Time: 837
LOW Column: (<""?k/cap) CAP
| % RELATIVEj ABUNDANCE
| 17,7f 46.2i 100,0j 6.6| 0,0{ 0.0)1I 95.6! 5.7( 5.9)1
176 | Greater than 95.0% but less than 101.0% of mass 174| 96. 2( .*/ )1 fj " <JG177 j 5.0 - 9.0% of mass 176 j 6.1( 6.3)2 fr'''
1 I1 -Value is % mass 174 2-Value is % mass 176
THIS TUNE APPLIES TO THE FOLLOWING SAMPLES, MS, MSD, BLANKS, AND STANDARDS:
| CLIENT | LAB| SAMPLE NO. | SAMPLE ID
31 | VSTD50 | VSTD50D2| VBLKLVXOBO-MB1 | 89LVX080-MB103 | SR-4-1-1MS | 8911L574-002S04 j SR-4-1-1MSD | 8911L574-002T05 j SR-4-1-2RE j 8911L574-00306 j, ]07| |08 1 !
"I I"I 114 1 115 1 I
18 1 |19| I201 I
I 1
LAB | DATEFILE ID | ANALYZED
AXBR02 | 11/27/89AXBR03. | 11/27/89AXBR14. | 11/27/89AXBR15. j 11/27/89AXBR16. j 11/27/89
1i1I1I1111It11I1
TIME |ANALYZED j— — i-•-»=--••--- 10914 |1005 j1631 |1759 11832 1
11111f11II11I1II
page 1 of 1 FORM V VOA 1/87 Rev.
fiR3Q3033
9PESTICIDE/PCS STANDARD SUMMARY
Lab Name: Rov F«.Weaton, Inc. Contract:
GC Sample ID: 12128903.27
Instrument IDs 23 ______ GC Column IDs 2250/2401
1J COMPOUND1
JAloha-BHC| Eeta-BHC|Delta-BHCI Qamny*— BHC (Lindane)JHeptachlor| Aldrin(Heptachlor epoxideJEndosulfan I| Dieldrin|4,4'-DDE(Endrin|Endosulfan II|4,4*-DDD|Endosulfan sulfate __|4,4*-DDT1 Methoxychlor(Endrin ketone| alpha-Chlordane| gamma-Chlordane| Toxaiahene|Aroclor-1016|Aroclor-1221|Aroclor-1232(Aroclor-1242 ,,,.„,„ „.| Aroelor-1248|Aroclor-1254lAroclor-1260., .I
| DATE(S) OF FROM: 12/12/89 - || ANALYSIS TO: 12/12/89 |j TIME(S) OF FROM: 1302 jj ANALYSIS TO: 1729 ji 1| | RT | i| RT | WINDOW | CALIBRATION |I | FROM | TO | FACTOR j* j .*..« | >«..« | »«« | »«««.Z3: || 1.74] 1.72] 1.76J 14555465J1 2.46| 2.44| 2.48) 5590411)1 2 .87 1 2 . 84 | 2 . 90 1 7270645 |1 2.19) 2.17| 2.21| 12280681)[ 2.67] 2.65| 2.69| 10832567]! 3 .22 | 3 . 18 | 3 . 24 | 8306253 |1 4.74| 4.69] 4.79| 6007393]1 5.94) 5.86) 6.00| 4648749 |J 7.22] 7.15| 7.29] 3803029)
1 6.70| 6.68| 6.72] 3808441].1 S.72| 8.63] 8.81] 2372243]| 10.49) 10.38) 10.60| 2565169)| 10.13] 10.11] 10.15] 2056649|J 16.36] 16.34) 16.38] 1562327]Jr 12.18] 12.16J 12.20J 1676913]| 22.79] 22.55] 23.03) 560583]| ******!****** | ****** | COELUTES *|
J, 5.70] 5.64) 5.76] 4463077)| 5.23] 5.18| 5.28] 4772801]| 10.70] 10.68] 10.72] 294885]| 2 .61 | 2 . 59 | 2 . 63 | 1804623 |J 1.60| 1.58] 1.62] 757922)_| 2.61| 2.59] 2.63] 990015]J 2 .61 | 2 . 59 | 2 . 63 | 1696589 |J 2.62| 2.60) 2.64] 1733149]_] 8.38) 8.35) 8.41] 1629277]J 9.40[ 9-38] 9.42] 968673]
] 1 1 1 1
DATE OF ANALYSIS 12/13/89 |TIME OF ANALYSIS 0952 IEPA SJ(STANI
RT
XKXC1SXS
2.162.663.214.735.927.20
10.47
12.1622.76
tMPLE NO. |)ARD) INDA 12-51 1
11 1 1
CALIBRATION |QNT| %D |FACTOR JY/N] |
13313849119008399166545718107951925154619223
2919861
1946707622037
iiiY | 8Y j '9Y j 10Y | 19Y | 11Y | 21
11
Y | 1311
Y j 16Y | 11
111111111111
"1111
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1•8|
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Under QNT Y/N: enter Y if quantisation was performed, N if not performed,%D mu*t be leas than or equal to 15.0% for quantitation, and leaa thanor equal to 20.0% for confirmation.
Note: Determining that no coapounds were found above the CRQL is a form ofquantitation, and therefore at least one column must meet the 15.0% criteria.
For nrulticomponent analytes, the single largest peak that is characteristicof the component should be used to establish retention time and %D.Identification of such analytes is based primarily on pattern recognition.
1 of _! FORM IX PEST 01/89 Rev.
9PESTICIDE/PCB STANDARD SUMMARY
Lab Name: Roy F. Weaton, Inc. Contracts
Case No.: ___________________ CC Sample ID: 12128903.42
RFW Lot No.: 8911L574
Instrument ID: 03______ GC Column ID: 2250/2401
I DATEfSl OF FROM: 12/12/89 I DATE OF ANALYSIS 12/13/b9j ANALYSIS TO: 12/12/89 j TIME OF ANALYSIS 1901j TIME<S) OF FROM: 3-302 | EPA SAMPLE NO.j ANALYSIS TOs 1729 j (STANDARD) IKDB 12-52
1| COMPOUND1
lAloha-BHC1 Beta-BBC|Delta-BHC| gamma-BHC { Lindane ) __| Heptachlor(Aldrin| Heptachlor epoxide(Endosulfan I(Dieldrin|4,4'-DDE| Endr in|£ndosulfan II|4,4'-DDD| Endosulfan sulfate ___|4,4'-DDT ..JMethoxychlor| Endr in ketone| alpha-Chlordane| qamma-Chlordane| Toxaphene|Aroclor-1016|Aroclor-1221(Aroclor-1232|Aroclor-1242(Aroclor-1248lAroclor-1254(Aroclor-12601
I| RT1|H__.| 1.74j 2.46j 2.87j 2.19j 2.67| 3.22| 4.74j 5.94| 7.22j 6.70| 8.72| 10.49j 10.13| 16.36j 12.18j 22.79j ******| 5.70| 5.23| 10.70| 2.61j 1.60| 2.61I 2.61| 2.62j 8.38I 9.40I
RT |WINDOW j
PROM | TO j==s=s=s: 1 ssss==s: j
1.72] 1.76|2.44) 2.48J2.84J 2.90J2.17J 2.21|2.65J 2.69|3.18| 3.24J4.69J 4.795.88J 6.00J7.15J 7.29|6,68) 6.72|8.63( 8.81J10.38J 10.60J10.11J 10.15|16.34J 16.38|12.16J 12.20|22.55J 23.03|****** I ****** j5.64) 5.765.18J 5.28|10.68J 10.72]2.59J 2.63|1,58| 1-^22.59J 2.63|2.59J 2.63|2.60J 2.64|8.35J 8.41J9.38J 9.42
1 1
1CALIBRATION |
FACTOR j=s=S3=KC==E=E* 1
14555465|5590411 |7270845 112280681 |10832567 j8306253)6007393 j4648749 |3803029J3808441 |2372243 j2565169 j2056649 j1562327 |1676913 |560583 j
COELUTES *|4463077)4772801)294885 j1804623 |757922)990015 |1696589 |1733149 |1629277)966673 j
1
RT
1-742.462.86
3.20
6.698.71
10,1216.34
5.695.22
1CALIBRATION |QNT
FACTOR JY/N«asssrs=s:==3==: ' —— ——
1489795554828517524397
8518093
37708632421397
19906091521209
42203394663655
1"--IT1 Y1 YIfI Y1111 YIY1I Y|Y11IYIY111111111 _
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2.41.93.5J
1' 12.6
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Under QNT Y/N: enter Y if quantisation was performed, N if not performed.%D must be less than or equal to 15.0% for guantitation, and less thanor ecjual to 20.0% for confirmation.
Note: Determining that no compounds were found above the CRQL is a form ofquantitation, and therefore at least one column must meet the 15.0% criteria.
For tculticomponent analytes, the single largest peak that is characteristicof the component should be used to establish retention time and %D.Identification of such analytes is based primarily on pattern recognition.page _2 of _S FORM IX PEST 01/89 Rev.
AR303Q35
5C9
PESTICIDE/PCB STANDARD SUMMARY
Lab Name: Sov F* Wegton, lac* Contract:
Case No.: _____________________ GC Sample ID: 12128903.57
RFW Lot No.: 8911L574
Instrument ID: W______ GC Column ID: 2250/2401
I DATS(S) OF FROM: 12/12/89 | DATE OF ANALYSIS 12/14/89j ANALYSIS TO: 12/12/89 | TIME OF ANALYSIS 0320j TIME(S) OF FROM: 1302 | EPA SAMPLE NO.| ANALYSIS TO: 1729 j (STANDARD) INDR 12-51
__________________!_____________________________I________________________| | RT | |
COMPOUND | RT | WINDOW (CALIBRATION] RT CALI BRAT ION |QNT| %Dj j FROM | TO I FACTOR j FACTOR JY/N)
|Alpha-BHC|Beta-BHC| Delta-BHC| gamma -BHC (Lindane)|H«ptachlor|Aldrin|Heptachlor epoxide ___JEndoaulfan I|Dieldrin|4.4'-DDE(Endrin|Endottulfan II]4.4'-DDD|Endoaulfan sulfate ___|4.4'-DDT.(MethoxYChlor|Endrin ketone| alpha-Chlordane] gamma-Chlordane|Toxaphene|Aroclor-1016|Aroclor-1221|Aroclor-1232|Aroclor-1242|Aroclor-1248|Ar oclor-1254]Aroclor-12601
•»—— - 11.74)2.46]2.87]2.19)2.67]3.22]4.74]5.94)7.22)6.70]8.72]10.49]10.13)16.36]12.18)22.79)****** I5.70|5.23110.70|2.61|1.60|2.61|2.61|2.62|8.38|9.401
!
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14555465]5590411]7270845)12280681) 2.1810832567] 2.668306253] 3.216007393] 4,734648749) 5.923803029] 7.203808441]2372243)2565169) 10.462056649]1562327]1676913] 12.15560583] 22.74
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Und«r QNT Y/K: enter Y if quantisation was performed, N if not performed%D must be leu than or equal to 15.0% for quantitation, and less thanor equal to 20.0% for confirmation.
Note: Determining that no compounds were found above the CRQL is a form ofquantitation, and therefore at least one column must meet the 15.0% criteria.
For multicomponent analytes, the single largest peak that is characteristicof the component should be used to establish retention time and %D.Identification of such analytes is based primarily on pattern recognition.
! _! FORM IX PEST 01/89 Rev.
AR303036
9 51PESTICIDE/PCB STANDARD SUMMARY
Lab Name: Rov F. Weston, Inc. _ , Contracts
Case No.: ___________________ GC Sample ID: 12128903.69
RFW Lot No.: 8911L574
Instrument ID; 03______ GC Column ID: 2250/2401
| DATE(S) OF FROM: 12/12/89 . \ DATE OF ANALYSIS 12/14/89I ANALYSIS TO: 12/12/89 j TIME OF ANALYSIS 0958j TIME(S) OF FROM: 1302 j EPA SAMPLE NO.j ANALYSIS TO: 1729 j (STANDARD) INDA 12-51
__________________I____________________________I________________________I I R I P I I I | |
COMPOUND I RT | WINDOW | CALIBRATION | RT (CALIBRATIONJQNT) %Dj I FROM | TO I FACTOR j j FACTOR JY/NJ
JAlpha-BHC___________! 1.74J 1.72J 1.76] 14555465 j |JBeta-BHC____________j 2.46) 2.44) 2.48J 5590411 j jJDelta-BHC___________| 2.87J 2.84J 2.90J 7270845) jjgamma-BHC (Lindane)__j 2.19) 2.17] 2.21J 12280681J 2.18) 12213333jHeptachlor_________j 2. 67 | 2.65 j 2.69 j 10832567 j 2.67 j 10318863JAldrin_____________j 3.22| 3,18) 3.24J 8306253J 3.21J 8054759j Heptachlor epoxide___ | 4.74 j 4.69 | 4.79 | 6007393| 4.741 5807465JEndosulfan I________j 5.94| 5.88) 6.00] 4648749j 5.93J 4484831JDieldrin___________1 7.22J 7.15) 7.29) 3803029 j 7.21) 3715489|4,4'~DDE____________I 6.70J 6.68J 6.72) 3808441) |JEndrin_____________j 8.72| 8.63J 8.81) 2372243) jJEndosulfan II_______j 10.49J 10.38) 10.60J 2565169) 10.48J 2540531|4,4'-DDD____________| 10.13) 10.11| 10.15) 2056649) |JEndosulfan sulfate___) 16.36] 16.34) 16.38) 1562327J j|4,4'-DDT____________j 12.18) 12.16J 12.20) 1676913] 12.17] 1687457JMethoxychlor________j 22.79] 22.55) 23.03] 560583] 22.78] 546835JEndrin ketone_______j******(******)******j COELUTES *| jj alpha-Chlordane_____ j 5.70) 5.641 5.76) 4463077 j |jgamma-Chlordane_____j 5.23) 5.18) 5.28] 4772801] jj.Toxaphene__________j 10.70] 10.68) 10.72) 294885) |JAroclor-1016________j 2.61) 2.59] 2.63) 1804623) |JAroclor-1221________j 1.60) 1.58] 1.62) 757922] |JAroclor-1232________j 2.61] 2.59] 2.63] 990015) ||Aroclor-1242________j 2.61) 2.59) 2.63] 1696589) jjj Aroclor-1248________ j 2.62 j 2.601 2.64 j 1733149 j |JAroclor-1254________j 8.38] 8.35) 8.41]' 1629277] |JAroclor-1260________| 9.40] 9.38) 9.42] 968673) j
0.5'4.73.03.33.52.3
0.62.5
Under QNT Y/N: enter Y if quantisation was performed, N if not performed.%D must be less than or equal to 15.0% for quantitation, and less thanor equal to 20.0% for confirmation.
Note: Determining that no compounds were found above the CRQL is a form ofquantitation, and therefore at least one column must meet the 15.0% criteria.
For multicomponent analytes, the single largest peak that ia characteristicof the component should be used to establish retention time and %D.Identification of such analytes is based primarily on pattern recognition.page _4 of _5 FORM IX PEST 01/89 Rev.
AR303037
9 .FESTICIDE/PCB STANDARD SUMMARY
Lab Name; Rov F» Weston* Inc» Contract:
Case No.: ___________________ GC Sample ID: 12128903.70
RFW Lot No.: 8911L574
Instrument ID: £3______ GC Column ID; 2250/2401
1j COMPOUHD1
|Alpha-BHC| Beta-BHC|Delta-BHC|gamma-BHC (Lindane)._..| Sept achlor|Aldrin(Heptachlor epoxide ___jlndosulfan IJDieldrin|4.4'-DDE|Bndrin|Endomulfan II|4.4'-DDD|Sndosulfan aulfate| 4 . 4 * -DDT| Methoxychlor|Endrin ketone| alpha-Chlordane| gamma-Chlordane| Toxaphene|Aroclor-1016|Aroclor-1221|Aroclor-1232| Aroclor-1242|Aroclor-124B|Aroclor-1254(Aroclor-1260 ,„..,., ,, ,1
| DATE(S) OF FROM: 12/12/89 • [| ANALYSIS TO: 12/12/89 |j TIME(S) OF FROM: 1302 j[ ANALYSIS TO: 1729 ji i| | RT | |1 RT | WINDOW | CALIBRATION]j j FROM | TO | FACTOR |
| 1.74J 1.72] 1.76] 14555465]j 2*46] 2.44] 2.48] 5590411]| 2. 87 1 2.84] 2.90] 7270845]j 2.19J 2.17] 2. 21 j 12280681]| 2.67] 2.65] 2.69] 10832567 jj 3.22] 3.18] 3.24] 8306253| 4.74J 4.69] 4.79] 6007393]j 5.94J 5.88] 6.00] 4648749]j 7.22] 7.15] 7. 29 1 3803029]j 6 . 70 1 6. 68 j 6.72 1 3808441 1| 8.72] 8.63J 8.81] 2372243]| 10.49] 10.38] 10.60] 2565169 |j 10.13] 10.11] 10.15J 2056649Jj 16.36] 16.34] 16.38] 1562327]j 12.1SJ 12.16] 12.20] 1676913]I 22.79) 22.55] 23.03J 560563]| ******]****** j ****** | COELUTES *|| 5.70J 5.64J 5.76] 4463077]j 5.23| 5.18] 5.28] 4772801J| 10.70J 10.68] 10.72] 294885]j 2.61] 2. 59 j 2.63] 1804623 |j 1.60 | 1.58J 1.62J 757922Jj 2.61J 2.59] 2.63J 990015j 2.61J 2.59] 2.63J 1696589]| 2.62J 2.60] 2.64] 1733149]| 8.38J 8.35] 8.41] 1629277 1j 9.40] 9.38J 9.42J 9686731 1 1 1 )
DATE OF ANALYSIS 12/14/89TIME CEPA SJ(STANI
RT
KSCKSCE
1.742.462.87
3.21
6.708.72
10.1316.35
5.705.23
)F ANALYSIS 1031UiPLE NO.>ARD1 INDB 12-52
1 1CALIBRATION |QNT| %D
FACTOR |Y/N|
1541265357748597908353
8919137
39557432530959
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Y | 5.9Y | 3.3Y | 8.8
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Y | 3.9Y i 6.7
1Y ] 7.6Y | 9.7
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Under QNT Y/N: enter Y if quantisation was performed, N if not performed.%D muat be less than or equal to 15.0% for quantitation, and less thanor equal to 20.0% for confirmation.
Note: Determining that no compounds were found above the CRQL is a form ofquantitationr and therefore at least one column must meet the 15.0% criteria.
For multicomponent analytes, the single largest peak that is characteristicof the component should be used to establish retention time and %D.Identification of such analytes is based primarily on pattern recognition.page _S of _JJ FORM IX PEST 01/89 Rev,
AR303038
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3R3Q3039
STAHDARD CHLORINECASE 89111,618
This quality assurance review is based upon a review of the datagenerated from six water and three soil samples collected on 11-27-89and analyzed by Roy F. Weston Lionville Analytical Laboratory for TCLVolatile and Semivolatile target compounds.
The reported analytical results are presented as a summary of the datain Section II. All of the analytical data were examined to determinethe usability of the analytical results and also to determinecontractual compliance relative to the analytical requirements anddeliverables specified in EPA's Contract Laboratory Program (CLP)protocol. Qualifier codes have been assigned next to the results sothat the data user can quickly assess the qualitative and/orquantitative reliability of any results.
Details of this quality assurance review are presented in the narrativesection of this report under each fraction. This report was prepared toprovide a critical review of the laboratory analyses and reportedanalytical results.
AR3030U
IREGARDING DATA
All data were reviewed according to CLP Functional Guidelines forEvaluating Organic Analyses. All data have been validated withregard to usability.
If you have any questions or comments on this data review, pleasecall Zohreh Hamid at (215)524-7360.
1. Attachment I - Glossary of Data Qualifier Codes.
2. Attachment II - Data Summary. This includes:
a) All positive results for the target analyteswith the qualifier codes, if applicable; and
b) All unusable detection limits (qualified "R") .
3. Attachment III - Re-submissions.
flR3030U2
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L618PAGE 2 OF 5
EVALUATION BY FRACTION
I I. Volatiles
Holding TimeSurrogate RecoveryMS/MSDBlankGC/MS TuningInitial CalibrationContinuing CalibrationCompound ID (HSL, TIC)StandardsSpectra QualityChroma tographyData Completeness
This portion of the case consisted of six water samples and three soilsamples which were analyzed according to CLP SOW 02/88 (Rev. 05/89) forTCL Volatile target compounds on 11-30-89, 12-01-89, and 01-08,17-90.
The problems with the analyses of the samples are addressed on anindividual sample basis. All general batch problems are listed afterthe samples.
SD-3-0-1. SD-3-0-1 MS, SD-3-0-2, SD-3-0-2-RE, SD-3-0-5, SD-3-0-5 RE
The 1,2-dichloroethane surrogate recoveries were above the EPA CLP QClimit of 121% and the chlorobenzene internal standard areas were belowthe control limit. Sample SD-3-0-5-RE also had the toluene surrogaterecovery exceed the EPA QC limit and all internal standards for SD-3-0-5and SD-3-0-5 RE were below EPA QC limits. The sample results may bebiased high; therefore, all guantitation limits and positive results arequalified estimated "J and UJ".
SW-3-0-1. SW-3-0-1 RE. SW-3-0-2, SW-3-0-5, SW-4-0-3. SD-4-0-3, SW-1-0-4
All water samples were extracted 35 days outside the EPA CLP QC holdingtime and the re-analysis of sample SW-1-0-4 was analyzed 44 days out ofholding time. Also, the toluene surrogate recoveries for SW-3-0-1, SW-4-0-3, SD-4-0-3, and VBLKLVB004-MB1 were below the EPA QC limit of 88.All positive results are rejected and the guantitation limits areconsidered estimated and flagged MUJ".
GENERAL -
The RRF for 2-butanone and 4-methyl-2-pentanone are below the EPA QClimit of 0.05 in the soil initial and continuing calibrations. Allassociated (juantitation limits are rejected and are flagged "R".
AR3Q30U3
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L618PAGE 3 OF 5
The soil laboratory blanks contain common contaminants methylenechloride and acetone at levels less than 3x the CRQL. The positiveresults that are less than lOx the blank level have the quantitationlimits adjusted to the value reported and 'are flagged "U". Themethylene chloride results which are greater than lOx the blankcontamination are considered true values. All of these results arestill flagged estimated due to other EPA criteria outliers.
Several compounds had %RSD and %D for initial and . continuingcalibrations exceed the 30 and 25% EPA QC limits. All positive resultsand guantitation have already been qualified due to other criteriaoutliers; no additional qualification is applied.
Several samples reported dichlorobenzene isomers as non-target compounds(TIC) while others did not. The representative positive results shouldbe obtained from the BNA fraction.
The % relative abundances for m/e = 176 on 11-14-89 at 7:19 and 12-01-89at 8:42 were not completely calculated. The corrected Forms V are re-submitted with this report.
The RRF 200 on the initial calibration on pi-11-9.0 was mislabeled asRRFSD2. The corrected Form VI is re-submitted.
All matrix spike recoveries were within EPA CLP QC limits.
IQA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L618PAGE 4 OF 5
EVALUATION B? FRACTION
II. Base/Heutral/Acids
x Holding Time___ Extraction Timex Surrogate Recoveryx Blank.JS_ MS/MSD___ GC/MS Tuningx Initial Calibrationx Continuing Calibration___ Compound ID (HSL, TIC)x Standards___ Spectra Quality___ Chromatography___ Data Completeness
This portion of the case consisted of five water samples and threesediment samples which were analyzed according to CLP SOW 02/88 (Rev.05/89) for TCL and client specified Semivolatile target compounds on 12-26-89, 01-04,18,22,23,25-90.
Samples SW-3-0-1, SW-3-0-5, SD-4-0-3, and SW-4-0-3 were analyzed 10-15days outside of the EPA CLP QC specified holding time- All associatedpositive results and quantitation limits are considered estimated andflagged "J and UJ".
Surrogate recovery criteria were not met for sample SD-3-0-2. Thesample was re-extracted outside the holding time; therefore the originalanalysis will be used. However, the results may be biased high;therefore, all positive results and quantitation limits are qualifiedestimated.
The chrysene and perylene internal standard areas were below controllimits for sample SW-3-0-5. This sample has already been qualified dueto the exceeded holding time; therefore, no additional qualification isapplied.
The soil blanks contain phenol, 1,4-dichlorobenzene, 1,2,4-trichlorobenzene, 1,2,4,5-tetrachlorobenzene at levels less than theCRQL. All positive results less than 5x the blank level have theguantitation limit adjusted to the value reported and are flagged "U".Positive results greater than 5x the blank contamination are consideredtrue values.
I QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L618PAGE 5 OF 5
The soil blank (89LE1203) also contained common contaminant di-n-butylphthalate at a level greater than 5x the CRQL- All associatedpositive results for this compound are rejected.
Several compounds had %RSD and %D in the' initial and continuingcalibrations exceed the 30% and 25% EPA CLP QC limits. Allcorresponding positive results and 'quantitation limits are qualifiedestimated »J and UJ".
The 4-nitrophenol matrix spike/spike duplicate recoveries (134/131)exceeded the EPA QC limit. This compound was not detected in theoriginal sample; therefore, these QC samples should not be used tojudge the long term precision and accuracy of the analytical method.Also, five of twenty-two blank spike recoveries are outside EPA QClimits. No qualification has been applied on this basis alone.
The p-terphenyl surrogate recovery exceeded the EPA QC limit in sampleSD-4-0-3; however, EPA surrogate criteria (i.e., no more than oneoutlier per fraction {acid and base neutral} and no recoveries less than10%), were met. No qualification is given.
The following nine client specified target compounds were librarysearched and several were detected in these samples:
aniline, n-nitrosodiphenylamine, benzidine,1,2,3-trichlorobenzene, 1,3,5-trichlorobenzene,1,2,4,5-tetrachlorobenzene, 1,2,3,4-tetrachlorobenzene•pentachlorobenzene, and l-chloro-3-nitrobenzene
Many unknown compounds were detected as Tentatively Identified Compounds(TIC's) in the soil samples.
GLOSSARY OF DATA QUALIFIERS
CODES RELATING TO IDENTIFICATION
(confidence concerning presence or absence of compounds):
0 « NOT DETECTED, SUBSTANTIALLY ABOVE THE LEVELREPORTED IN LABORATORY OR FIELD BLANKS.
R = UNRELIABLE RESULT. ANALYTE MAY OR MAY NOT BEPRESENT IN THE SAMPLE. SUPPORTING DATANECESSARY TO CONFIRM RESULT.
N = NEGATED COMPOUND WAS CONSIDERED AS NOTPRESENT IN THE SAMPLE.
(NO CODE) = CONFIRMED IDENTIFICATION
CODES RELATING TO QtTANTITATION
(can be used for both positive results and sample quantitationlimits):
J = ANALYTE PRESENT. REPORTED VALUE MAY NOT BEACCURATE OR PRECISE.
DJ = THE REPORTED QUANTITATION LIMITS AREQUALIFIED ESTIMATED.
OTHER CODES
NO ANALYTICAL RESULT.
5R3030U8
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VOLATILE ORGANIC GC/KS TUNING AND MASS f 18CALIBRATION - BROMOFLUOROBENZENE (BFB)_
Lab Name: Hoy F* Weston, Ing* Contracts 2267-09-02-0000
Case Ho.: STAHDAR5 CISiORINE______
Lab File IDs AXBE01 • BFB Injection Dates 11/14/B9
Instrument ID: S>-HSO X BFB Injection Times _719
Matrix: (soil/water) SOIL Level: (low/med) £OW , Columns (pack/cap) CAP
Im/« | ION ABUNDANCE CRITERIA
SO759596173174175176177
15.0 - 40.0% of mass 9530.0 - 60.0% of mass 95Base peak, 100% relative abundance5.0 - 9*0% of mass 95Less than 2.0% of mass 174Greater than 50.0% of mass 955.0 - 9.0% of mass 174Greater than 95.0% but less than 101.0% of mass 1745.0 - 9.0% of mass 176
'
% RELATIVEABUNDANCE
18.950.1100.06.70.0{77.35.5(77. 4{ /5.7(
0.0)1
7.2)1
7.4)2
1-Value is % mass 174 2-Value is % mass 176
THIS TUNE APPLIES TO THE FOLLOWING SAMPLES, MS, MSD, BLANKS, AND STANDARDS:
CLIENT | LAB | LAB | DATESAMPLE NO. SAMPLE ID PILE ID ANALYZED
01 1 VSTD20 | VSTD20 | AXBE02 | 11/14/8902 | VSTD50 ~~ | VSTD50 j AXBE03 | 11/14/8903 | VSTD100 I VSTD100 | AXBE04 j 11/14/8904 1 VSTD150 I VSTD1SO j AXBE05 j 11/14/8905 | VSTD200 | VSTD200 j AXBE06 | 11/14/890 6 | I I I0 7 | I I Io a | 1 1 10 9 | I l li o | I I In| I I I12 1 I I I« | I I I1 4 I I I I" I I I I16 1 I I I
~
"I201
TIMEANALYZED
08170849092009521024
page 1 of 1 FORM V VOA 1/87 Rev.
SR30306
5A 20VOLATILE ORGANIC GC/MS TUNING AND MASSCALIBRATION - BROMOFL0OROBENZENE (BFB)
Lab Name: Roy F. Weaton, Inc. Contract: 2267-09*02-0000
Cafle NO.: STANDARD CHLORINE______
Lab Pile ID: AXC101 • BFB Injection Date: 12/01/69
Instrument ID: HP-MSD I BFB Injection Time* 342
Matrix: (soil/water) SOIL Levels(low/med) LOW Column: (pack/cap) CAP
m/e
50759596173174175176177
ION ABUNDANCE CRITERIA
15.0 - 40.0% of mass 9530.0 - 60.0% of mass 95Base peak, 100% relative abundance5.0 - 9.0% of mass 95Less than 2.0% of mass 174Greater than 50.0% of mass 955.0 - 9.0% of mass 174Greater than 95.0% but less than 101.0% of mass 1745.0 - 9.0% of mass 176
% RELA1ABUNDJ
17.050.5100.06.20.0(
90.45.2(91. 0(,6.0(
rivEiNCE
0.0)1
5.8)100.7)16,6)2| *•••"
1-Value is % mass 174 2-Value is % mass 176
THIS TUNE APPLIES TO THE FOLLOWING SAMPLES, MS, MSD, BLANKS, AND STANDARDS:
I CLIENT | LAB | LAB | DATE TIMEj SAMPLE NO. | SAMPLE ID | FILE ID | ANALYZED ANALYZEDI »«s«jr Esss=s==r=:s=s =s=:s:=s;s=s I e=ss=sj=s:sss:s=s:e:=: I Es=sssaeaxs=ss=s; I KxsaEBSxxata
01 1 VSTD50 j VSTDSO | AXC102 | 12/01/89 090702 1 VBLKLVX084-MB1 | 89LVX084-MB1 | AXC103. | 12/01/89 095503 j SD-3-0-1MSD j 8911L618-003T | AXC104. | 12/01/89 111404 1 SD-3-0-2RE j 8911L618-004 | AXC105. j 12/01/89 114605 1 SD-3-0-5RE I 8911L618-005 | AXC106. | 12/01/89 121806 | I I I0 7 | I I I0 8 | I I I0 9 1 I I I1 0 | I I IHI I I I1 2 | I I I" I I I I" I I I I1S
"I"I20|
page 1 of 1 FORM V VOA 1/87 Rev.
4R303062
VOIATILS ORGANICS INTITIAL CALIBRATION DATA
Lab Name: ftov F» Wegton, Inc» Contracts 2267 09-02-0000
Case No.: STANPABP CHLORIHS______ RFW Lot: 893.1L618
ln»trument ID* S1QQB Calibration Date(s): 01/11/90 01/11/90
Matrix :(ioil/water) WATER Level:(low/med) LOW Column: (pack/cap) CAP
Min iS* for SPCC(f) * 0.300 (0.250 for Bromoform) ' Max %RSD for CCC(*> » 30.0%
|IAB FILE ID: *R«D2« BQ11105 RRP20 » B011106|RRF so* 1011102 v'V RRFIOO- EQUIPS RRFISO* BO 111041| |/*/Voej COMIKDOiro (Jffl SOS
j Chlorome thane f 0.643| Bromomethane ! 0.888| Vinyl Chloride * 0.725| Chloroethane | 0.658|M*thYl*ne Chloride | 1.185(Acetone 1 0.676(Carbon Diaulfide | 2.4181 1 - 1-Dichloroethene * 1 . 068|l,l-Dichloro«thane * 2.773|l,2-Dichloroethene (total) ___ |(Chloroform , * 3.244|1.2-Dichloroethane ) 0.460|2-Butanon@ 1 0.1231 1 r 1 f 1-Trichloroethane ,. | 2.297(Carbon Tetrachloride. , . _ I 2.002(Vinvl Acetate | 0.34S( Bromodichlorocaethane | 0.717| lP2-Dichloropropan© * 0.395|ci«-l,3-Dichloropropene, | 0.551|Trichloroethene | 0.363jDibromochlorooethane | 0.5841 1P lf 2-Trichloroethan@ | 0.365(Benzene | 0.896| Trann-1 , 3-Dichloropropene ___ | 0 . 677| Bromoform ,,, 1 0.4311 4-Methyl-2-pentanone | 0.224| 2-Hexanone | 0.293| Tetrachloroethene | 0.378(1,1,2, 2-Tetrachloroethane ____ f 0 . 618(Toluene * O.S87| Chlorobenzene * 0.967[Ethvlbenzene * 0.477(Stvrene 1 1.078[Xylcne ( total 1 || w:iKKKXMKHXsac«tK»*2tmaE:x:Bcae8ESEm:£;Es=ssEs?£;:sE«=
|Toluene-d8 | 1.100| Broraof luorobenzene ( 1.0251 1 , 2-Dichloroethane-d4 | 0 . 4981 !
RRF20
1.0301.2361.0671.0772.3680.8693.1111.1633.194
3.9490.5320.2332.8572.6820.3870.8830.4680.7000.4720.7110.4171.0280.9350.5980.3010.4370.5260.7920.6161.0950.4711.010
1.6021.1370.581
1RRP so IRRFIOO0.9321.0790.9640.8951.7480*850
•T 2.5471.2712.972
3.5310.4860.1212.3162.1110.3880.7790.4090.5770.4130.6590.3950.9560.7820.4990.2910.4020.4640.7080.8601.0130.4961.022
1.4231.0270.533
0.8641.1210.9860.7311.3610.8252.4661.1432.976
3.4870.4950.1422.4752.1790.3780.7740.4140.5850.3930,6610.4010.9610.7560.5080.2680.3890.4380.7030.8701.0290.4871.128
£2KKeS5=Ka
1.3471.1090.539
RRF150
0.7641.0400.7900.8171.2060.8042.4261.0772.925
3.3690.5070.1292.3542.0890.3730.7710.4260.6060.3860.6600.4110.9570.7660.4850.2640.3370.4320.6980.6791.0480.5101.180
BSEKeSBES
1.2631.0980.522
RRF
0.8471.0730.9100.8361.5740.8052.5941.1442.968
3.5160.4960.1502.4602.2130.3740.7850.4220.6040.4060.6550.3980.9640.7830.5040.2700.3720.4480.7040.7631.0300.4881.084
£&3E»eCXl
1,3471.0790.535
* 1RSD |
————— 117. 7#11. 9|16.0*19.4)31.719.5|11.317.1*5. If
'.:j|31. 6|9.5)12. 2|4.717.7)6.6*9.5)10.1|6.9]5.115.0|12. 0|12. Otll.lj15. 3J12, 0|8.8*16.3*4.6t3.2*6,6|
1C3C3XX3C 1
13. M4.15.71
1FORM VI VOA 01/89 Rev.
AR3Q3063
STANDARD CHLORINECASE 89111.628
This quality assurance review is based upon a review of the datagenerated from one water sample collected on 11-28-89 and analyzedby Roy F. Weston Lionville Analytical Laboratory for TCL Volatiletarget compounds.
The reported analytical results are presented as a summary of thedata in Section II. All of the analytical data were examined todetermine the usability of the analytical results and also todetermine contractual compliance relative to the analyticalrequirements and deliverables specified in EPA's ContractLaboratory Program (CLP) protocol. Qualifier codes have beenassigned next to the results so that the data user can quicklyassess the qualitative and/or quantitative reliability of anyresults.
Details of this quality assurance review are presented in thenarrative section of this report under each fraction. This reportwas prepared to provide a critical review of the laboratoryanalyses and reported analytical results.
\
INFORMATION REGARDING DATA
All data were reviewed according to CLP Functional Guidelines forEvaluating Organic Analyses. All data have been validated withregard to usability.
If you have any questions or comments on this data review, pleasecall Zohreh Hamid at (215)524-7360.
ATTACHMENTS
1. Attachment I - Glossary of Data Qualifier Codes.
2. Attachment II - Data Summary. This includes:
a) All positive results for the target analyteswith the qualifier codes, if applicable; and
b) All unusable detection limits (qualified "R") .
BR303065
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L628PAGE 2 OF 2
EVALUATION BY FRACTION
I. Volatiles
Holding TimeSurrogate RecoveryMS/MSDBlankGC/MS TuningInitial CalibrationContinuing CalibrationCompound ID (HSL, TIC)Standards.Spectra QualityChromatographyData Completeness
This portion of the case consisted of one water sample which wasanalyzed according to CLP SOW 02/88 (Rev. 05/89) for TCL Volatiletarget compounds on 11-30-89.
The response factors for 2-butanone and 4-methyl-2-pentanone in theinitial and continuing calibrations were below the EPA QC limit of0.05. The associated guantitation limits are rejected and flagged"R" in the data summary.
The laboratory blank contained common contaminant methylenechloride at a level less than the CRQL. The sample result is lessthan lOx the blank contamination; therefore, the guantitation limitis adjusted to the value reported and flagged "U".
Several compounds had %RSD and %D for initial and continuingcalibrations exceed the 30% and 25% EPA QC limits. All associatedguantitation are qualified estimated "UJ".
Sample SW-8-0-4-MS had the 1,2-dichloroethane surrogate recoveryexceed the EPA QC limit of 114%. Also the bromochloromethaneinternal standard area was below the control limits. Results maybe biased high; therefore, they are considered estimated.
All matrix spike recoveries are within EPA QC limits.
ftR3Q3Q66
\
GLOSSARY OF DATA QUALIFIERS
CODES RELATING TO IDENTIFICATION
(confidence concerning presence or absence of compounds)
0 = NOT DETECTED, SUBSTANTIALLY ABOVE THE LEVELREPORTED IN LABORATORY OR FIELD BLANKS.
R = UNRELIABLE RESULT. ANALYTE MAY OR MAY NOT BEPRESENT IN THE SAMPLE. SUPPORTING DATANECESSARY TO CONFIRM RESULT.
N = NEGATED COMPOUND WAS CONSIDERED AS NOTPRESENT IN THE SAMPLE.
(NO CODE) = CONFIRMED IDENTIFICATION
CODES RELATING TO QtJANTITATION
(can be used for both positive results and sample guantitationlimits):
J = "ANALYTE PRESENT. REPORTED VALUE MAY NOT BEACCURATE OR PRECISE.
UJ = THE REPORTED QUANTITATION LIMITS AREQUALIFIED ESTIMATED.
OTHER CODES
NO ANALYTICAL RESULT.
SR3Q3Q68
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STANDARD CHLOStXNBCASE 8911L636 (VOA, BHA, PEST/PCB)
CASE 89111.618 (PEST/PCB)
This quality assurance review is based upon a review of the datagenerated from six water samples and six soil samples collected on11-27,29-89 and analyzed by Roy F. Weston Lionville AnalyticalLaboratory for TCL Volatile, Semivolatile, and Pesticide/PCB(8911L636 and 8911L618) target compounds.
The reported analytical results are presented as a summary of thedata in Section II. All of the analytical data were examined todetermine the usability of the analytical results and also todetermine contractual compliance relative to the analyticalrequirements and deliverables specified in EPA's ContractLaboratory Program (CLP) protocol. Qualifier codes have beenassigned next to the results so that the data user can quicklyassess the qualitative and/or quantitative reliability of anyresults.
Details of this quality assurance review are presented in thenarrative section of this report under each fraction. This reportwas prepared to provide a critical review of the laboratoryanalyses and reported analytical results.
AR3Q3Q72
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L636/618PAGE 2 OF 7
EVALUATION BY FRACTION
I. VQlatil.es
___ Holding Timex Surrogate Recoveryx MS/MSDx Blank___ GC/MS Tuningx Initial Calibrationx Continuing Calibration___ Compound ID (HSL, TIC)x Standards___ Spectra Quality___ Chromatographyx Data Completeness
This portion of the case consisted of two water and three soilsamples which were analyzed according to CLP SOW 02/88 (Rev. 05/89)for TCL volatile target compounds on 12-04,06,07-89.
The 2-butanone response factor in the soil initial and continuingcalibrations and 4-methyl-2-pentanone response factor in the waterinitial and continuing calibrations were less than the 0.05 EPA CLPQC limit. The quantitation limits for these compounds are rejectedand are flagged "R" in the data summary.
The following samples had surrogate recoveries below the EPA CLP QClimits.
Sample Surrogate
BS-1-0-1 TolueneBS-1-0-1MS TolueneBS-1-0-1MSD TolueneBS-1-0-2 All SurrogatesBS-1-0-2RE Toluene, BromofluorobenzeneBS-l-0-5 Toluene, BromofluorobenzeneBS-1-0-5RE Toluene
EPA surrogate criteria were not met for the above samples. Allpositive results and quantitation limits are considered estimated.
In the case of sample BS-1-0-2, all of the internal standard areaswere also below the control limits. The reanalysis had no internalstandard outliers, therefore, the re-analysis is to be used as therepresentative sample with the applied qualifier codes due to thesurrogate outliers.
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L636/618PAGE 3 OF 7
( T h e laboratory blanks contain common contaminants methylenechloride and acetone at levels less than 5X the CRQL. Allassociated positive results less than 10X the blank level have thequantitation limits adjusted to the reported value and are flagged"U" in the data summary. The methyiene chloride result (130 ug/L)in sample BS-1-0-3 was .above 10X the associated blank level;therefore, it is considered a true value.
Several compounds had %RSD and %D in the water initial andcontinuing calibrations exceed the 30 and 25% EPA CLP QC limit.All associated positive results and quantitation limits areconsidered estimated and are flagged "J" and "UJ", respectively.
The 1,1-dichloroethene matrix spike/spike duplicate recoveries arebelow the EPA CLP QC limit (59%). Matrix spike recoveries are onlyused as a guideline to judge the long term precision and accuracyof the analytical method; therefore, no qualification is applied."
The Form I-TICs were missing from the re-analyses.
Dichlorobenzene was detected as a non-target compound in mostsamples.
AR30307U
I
Ii
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L636/618PAGE 4 OF 7
EVALUATION BY FRACTION
II. Base/Neutral/Acids
x Holding Time___ Extraction Time___ Surrogate Recoveryx Blank___ MS/MSDx GC/MS Tuningx Initial Calibrationx Continuing Calibration___ Compound ID (HSL, TIC)x Standards___ Spectra Quality___ Chromatography___ Data Completeness
This portion of the case consisted of one water and three soilsamples which were analyzed according to CLP SOW 02/88 (Rev. 05/89)for TCL and client specified semivolatile target compounds on12-31-89 and 01-04,05,06,08,09,23-90.
The following samples required dilution due to high levels ofchlorobenzene compounds.
Sample Dilution Factor
BS-1-0-1 5:55/1110BS-1-0-2 111BS-1-0-5 5:55/1110 _.
The diluted results are only to be used for those compounds thatexceeded the calibration range in the original analysis, all otherresults come from the original analysis. The surrogate recoverieswere not able to be obtained due to these dilutions.
Sample BS-l-0-3 was analyzed fourteen days outside the analysisholding time. Therefore all positive results and quantitationlimits are qualified estimated and are flagged "J11 and "UJ" in thedata.
The analysis of samples BS-l-O-l DL (16 minutes) and BS-l-0-5 DL (1hour, 3 minutes) exceeded the 12-hour analysis tune criteria forthe tune performed on 01-05-90 at 14:39 on the 5100M. Thereforethe reported results may be biased, and are considered estimatedand flagged "J" in the data summary.
RR303075
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L636/618PAGE 5 OF 7
The following internal standard areas are below the control limits.
Sample Internal.Standard
BS-l-O-l 1,4-DichlorobenzeneBS-1-0-2 1,4-DichlorobenzeneBS-1-0-5 All StandardsBS-1-0-1DL 1,4-Dichlorobenzene,
Naphthalene
The positive results are probably biased high; therefore, they areconsidered estimated and are flagged "J".
Seven of 22 blank spike recoveries are outside EPA QC limits. Noqualification is applied on this basis alone, since spikerecoveries are only used to judge the long term precision andaccuracy of the data.
Several compounds had %RSD and %D in the initial and continuingcalibrations exceed the 30 and 25% EPA CLP QC limits. The affectedsamples BS-l-O-l, BS-1-0-2, and BS-1-0-5 have the associatedcompound quantitation limits qualified estimated and flagged "UJ11in the data summary.
The soil blank has di-n-butylphthalate at a level greater than 5Xthe CRQL; therefore, the associated sample results are consideredbiased high and are flagged "U" in the data summary. This blankalso contains several other target compounds at levels less thanthe CRQL. The only positive result less than 5X the blank level isthe phenol value for sample BS-1-0-5. This sample has thequantitation limit adjusted to this reported value and is flagged"U" in the data summary. All other results are greater than 5X theblank contamination and are considered true values.
The water blank has di-n-butylphthalate at a level less than theCRQL. The associated positive result is less than 5X the blanklevel; therefore, the quantitation limit is adjusted to thereported value and is flagged "U".
The following nine client specified compounds were library searchedand many were detected in these samples: aniline, n-nitroso-diphenylamine, benzidine, 1,2,3-trichlorobenzene, 1,2,5-trichloro-benzene, 1,2,4,5-tetrachlorobenzene, 1,2,3,4-tetrachlorobenzene,pentachlorobenzene and l-chloro-3-nitrobenzene.
Many unknown and chlorobenzene compounds were detected in thesesamples as Tentatively Identified Compounds (Tie's).
SR3Q3076
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L636/618PAGE 6 OF 7
EVALUATION BY FRACTION
III. Pesticides/PCB
x Holding Time___ Extraction Timex Surrogate Recovery_x_ MS/MSDx Blank___ Linearity Calibration___ DPT/Endrin Degradation___ Analytical Sequence___ DEC Retention Timex Continuing Calibrationx Retention Time Window___ Standards___ Chromatography___ HSL Compounds___ Data Completeness
This portion of the cases consisted of 6 water and 6 sedimentsamples which were analyzed for TCL Pesticide/PCB target compoundson 12-18,19-89 and 01-09,10-90.
Samples SD-3-0-5/MS/MSD, BS-1-0-1, BS-1-0-2, and BS-l-O-S wereanalyzed one day outside the EPA CLP holding time. No positiveresults were found in these samples and since holding time is anadvisory limit, no qualification is applied.
Blank (89LE1200-MB1) contained 4,4,-DDT (0.020 ug/L) at a levelless than the CRQL. This compound was detected in associatedsample SW-3-0-5 at a level less than the CRQL. Since the reportedresult in this sample is less than 5X the blank level, thequantitation limit is qualified "U" and should be considered notpresent in the sample.
The following samples required dilution because they contained highlevels of early eluting compounds.
Sample Dilution Factori
SD-3-0-1 5SD-3-0-2 5SD-3-0-5/MS/MSD 5BS-1-0-1 50BS-1-0-2 50BS-1-0-5 50BS-1-0-3 10
AR303077
Iri
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8911L636/618PAGE 7 OF 7
Surrogate recoveries could not be obtained for samples BS-l-0-1,BS-l-o-2, and BS-1-0-5 due to the required dilution.
The surrogate recoveries for samples SD-3-0-5 and its matrixspike/spike duplicate exceeded the advisory QC limits. Sincepositive results were not detected in these samples, noqualification has been applied.
The matrix spike/spike duplicate recoveries for gamma-BHC in sampleSD-3-0-5 could not be obtained due to interference of non-targetcompounds. There is no impact to the data since this compound wasnot detected in the samples.
The first two IND A and IND B were outside the calibration range(12-19-89 at 08:32 and 09:05). Corrective action was taken andthey were reanalyzed (12-19-89 at 11:14 and 11:47) with nocalibration problems.
The %D on the primary column analyzed on 12-18,19-89 and 01-09,ID-89 for delta-BHC, alpha-chlordane, gamma-chlordane (IND B 12-19-89at 09:05), 4,4-DDT (IND A 12-19-89 at 11:14), 4,4-DDT (IND A 01-10-90 at 05:06), aldrin (IND B 01-10-90 at 14:23), heptachlor epoxide(IND A 01-10-90 at 14:56) exceeded the 15% requirements limits.These compounds were not detected in the samples; therefore, thereis no impact to the data.
Also, ,%D for up to six compounds exceeded the 20% requirement forthe confirmation column. Once again no qualification was applied,since there were no .positive target compound results.
The retention times were outside the established window on theconfirmation column for 4,4,-DDE, endrin, (IND B 12-19-89 at09:07), endosulfan II, 4,4-DDT, methoxychlor (IND A 12-19-89 at11:16), 4,4-DDE, endrin, 4,4-DDD, endrin ketone (IND B 12-19-89 at11:49), 4,4-DDE, endrin, 4,4-DDD, endrin ketone (IND B 12-19-89 at19:39) dieldrin, endosulfan II, 4,4-DDT, methoxychlor (IND A 12-20-89 at 02:16) and 4,4-DDE, endrin, 4,4-DDD, endosulfan sulfate,endrin ketone (IND B 12-20-89 at 11:07). The data is not affectedsince these compounds were not detected in the samples.
flR303078
INFORMATION REGARDING DATA
All data were reviewed according to EPA CLP Functional Guidelinesfor Evaluating Organic Analyses. All data have been validated withregard to usability,
If you have any questions or comments on this data review, pleasecall Zohreh Hamid at (215)524-7360.
ATTACHMENTS 7 ——_.._..,,_.__—
1. Glossary of Data Qualifier Codes.
2. Data Summary. This includes:
a) All positive results for the target analyteswith the qualifier codes, if applicable; and
b) All unusable detection limits (qualified "R") .
3. Support Documentation includes details to support thestatements in this reports.
5R303079
COPES RELATING TO IDENTIFICATION
(confidence concerning presence or absence of compounds)
U = NOT DETECTED, SUBSTANTIALLY ABOVE THE LEVELREPORTED IN LABORATORY OR FIELD BLANKS.
R = UNRELIABLE RESULT. ANALYTE MAY OR MAY NOT BEPRESENT IN THE SAMPLE. SUPPORTING DATANECESSARY TO CONFIRM RESULT.
N = NEGATED COMPOUND WAS CONSIDERED AS NOTPRESENT IN THE SAMPLE.
(NO CODE) = CONFIRMED IDENTIFICATION
CODES RELATING TO QUANTITATION .. -
(can be used for both positive results and sample guantitationlimits):
J = ANALYTE PRESENT. REPORTED VALUE MAY NOT BEACCURATE OR PRECISE.
UJ = THE REPORTED QUANTITATION LIMITS AREQUALIFIED ESTIMATED.
OTHER CODES
NO ANALYTICAL RESULT.
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WESTON ANALYTICS
PESTICIDE/PCB'sCLP
LIST
III
STANDARD CHLORINECASE 8912L749
This quality assurance review is based upon a review of the datagenerated from two water and three soil samples collected on12-06-89 and analyzed by Roy F. Weston Lionville AnalyticalLaboratory for TCL Volatile and Semivolatile target compounds.
The reported analytical results are presented as a summary of thedata in Section II. All of the analytical data were examined todetermine the usability of the analytical results and also todetermine contractual compliance relative to the analyticalrequirements and deliverables specified in EPA's ContractLaboratory Program (CLP) protocol. Qualifier codes have beenassigned next to the results so that the data user can quicklyassess the qualitative and/or quantitative reliability of anyresults.
Details of this quality assurance review are presented in thenarrative section of this report under each fraction. This reportwas prepared to provide a critical review of the laboratoryanalyses and reported analytical results.
AR303090
* INFORMATION REGARDING DATA
All data were reviewed according to CLP Functional Guidelines forEvaluating Organic Analyses. All data have been validated withregard to usability.
If you have any questions or comments on this data review, pleasecall Zohreh Hamid at (215)524-7360.
ATTACHMENTS
1. Attachment I - Glossary of Data Qualifier Codes.
2. Attachment II - Data Summary. This includes:
a) All positive results for the target analyteswith the qualifier codes, if applicable? and
b) All unusable detection limits (qualified "R") .
flR30309i
iQA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8912L749PAGE 2 OF 5
EVALUATION BY FRACTION
I* Volatiles
Holding TimeSurrogate RecoveryMS/MSDBlankGC/MS TuningInitial CalibrationContinuing CalibrationCompound ID (HSL, TIC)StandardsSpectra Quality
___ Chromatography___ Data Completeness
This portion of the case consisted of two waters and three soilsamples which were analyzed according to CLP SOW 02/88 (Rev. 05/89)for TCL Volatile target compounds on 12-11,12-89.
The toluene surrogate recovery for sample SS-6-1-4 (86%) was belowthe EPA QC limit of 88. The sample was not re-analyzed and theresults may be biased low; therefore, all positive results andguantitation limits are considered estimated and flagged "J andUJ". The sample was also missing the library search for targetcompound benzene.
The response factors for 2-butanone and vinyl acetate for the soilinitial and continuing calibrations were below the EPA QC limit of0.05 in the initial and continuing calibrations. The associatedguantitation limits are rejected and are flagged "R" in the datasummary.The soil laboratory blanks contain common contaminant methylenechloride at levels less than 2x the CRQL. The correspondingsamples contain this compound at levels less than lOx the blankcontamination. Therefore, the quantitation have been adjusted tothe level of value reported and flagged with a "U".
Several compounds had %RSD and %D in initial and continuingcalibrations exceed the 30% and 25% EPA QC limits. All associatedpositive results and guantitation limits are gualified estimated "Jand UJ", respectively.
flR303D92
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8912L749PAGE 3 OF 5
Sample SS-13-1-5 MSD matrix spike recovery for Benzene (158%) wasabove the EPA QC limit of 142%. The original sample and QC samplescontain significant amounts of this compound that may interferewith the spike recovery result. Also, the chlorobenzene internalstandard area was below the control limit for this QC sample.Therefore, results may be biased high; the data should beconsidered estimated.
flR303093
III
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8912L749PAGE 4 OF 5
EVALUATION BY FRACTION
II* Base/Neutral/Acids
___ Holding Time___ Extraction Time___ Surrogate Recoveryx BlankX MS/MSD___ GC/MS Tuningx Initial Calibrationx Continuing Calibration___ Compound ID (HSL, TIC)___ Standards___ Spectra Quality___ Chromatography___ Data Completeness
This portion of the case consisted on one water and three soilsamples which were analyzed according to CLP SOW 02/88 (Rev. 05/89)for TCL and client specified Semivolatile target compounds.
Several compounds had %RSD and %D in the initial and continuingcalibrations exceed the 30% and 25% EPA CLP QC limits. Allassociated positive results and quantitation limits are qualifiedestimated and flagged "J" and UJ" in the data summary,
The soil laboratory blank (89LE1274) contained benzoic acid and di-n-butylphthalate at levels less than the CRQL. For benzoic acid,the positive results for .samples SS-13-1-1 and SS-13-1-5 were lessthan 5x the blank level; therefore, the quantitation limits areadjusted to the value reported and are flagged "U". The result forsample SS-13-1-2 was above 5x the blank contamination, it isconsidered a true value. In the case of di-n-butylphthalate, allsoil positive results were less than lOx the blank level; onceagain, the quantitation limits are adjusted to the level of thevalue reported and are flagged "Un.
The matrix spike/spike duplicate recoveries for 1,2,4-trichloro-benzene in sample SS-13-1-1 were outside EPA CLP QC limits(0%/476%). The QC results differed significantly; however, theoriginal sample contained a high level of this compound.Therefore, the matrix spike recoveries should not be used to judgethe long term precision and accuracy of the analytical method.Also, all blank spike recoveries were within EPA CLP QC limits. Noqualification is applied on this basis alone.
AR303091*
I QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8912L749PAGE 5 OF 5
The following nine client specified target compounds were librarysearched and several were detected in these samples:
aniline, n-nitrosodiphenylamine, benzidine,1,2,3-trichlorobenzene, 1,3,5-trichlorobenzene,1,2,4 r5-tetrachlorobenzene, 1,2,3,4-tetrachlorobenzenepentachlorobenzene, and l-chloro-3-nitrobenzene
Many unknown compounds were detected as Tentatively IdentifiedCompounds (Tie's) in the soil samples. Several of the samecompounds were detected in the associated blank; those specificcompounds could be a result of laboratory contamination.
flR303095
L GLOSSARY OF DATA QUALIFIERS
CODES RELATING TO IDENTIFICATION
(confidence concerning presence or absence of compounds)
U = NOT DETECTED, SUBSTANTIALLY ABOVE THE LEVELREPORTED IN LABORATORY OR FIELD BLANKS.
R = UNRELIABLE RESULT. ANALYTE MAY OR MAY NOT BEPRESENT IN THE SAMPLE. SUPPORTING DATANECESSARY TO CONFIRM RESULT.
N = NEGATED COMPOUND WAS CONSIDERED AS NOTPRESENT IN THE SAMPLE.
(NO CODE) = CONFIRMED IDENTIFICATION
CODES RELATING TO OUANTITATION
(can be used for both positive results and sample guantitationlimits):
J = ANALYTE PRESENT. REPORTED VALUE MAY NOT BEACCURATE OR PRECISE.
DJ = THE REPORTED QUANTITATION LIMITS AREQUALIFIED ESTIMATED.
OTHER CODES
NO ANALYTICAL RESULT.
flR303097
STANDARD CHLORINET2ABE 8912L698 (VOA, BNA, AHD PEST/PCB)
CASE 89121*749,768 (PEST/PCB ONLY)
This quality assurance review is based upon a review of the datagenerated from six water samples and six sediment samplescollected on 12-04,06,07-89 and analyzed by Roy F. Weston LionvilleAnalytical Laboratory for TCL Volatile/ Semivolatile, andPesticide/PCB target compounds.
The reported analytical results are presented as a summary of thedata in Section II. All of the analytical data were examined todetermine the usability of the analytical results and also todetermine contractual compliance relative to the analyticalrequirements and deliverables specified in EPA's ContractLaboratory Program (CLP) protocol. Qualifier codes have beenassigned next to the results so that the data user can quicklyassess the qualitative and/or quantitative reliability of anyresults.
Details of this quality assurance review are presented in thenarrative section of this report under each fraction. This reportwas prepared to provide a critical review of the laboratoryanalyses and reported analytical results.
AR303099
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASES 8912L698,749,768PAGE 2 OF 7
EVALUATION BY FRACTION
I. Volatiles
___ Holding Timex Surrogate RecoveryX MS/MSD_£_ Blankx GC/MS Tuning_j£_ Initial Calibrationx Continuing Calibration___ Compound ID (HSL, TIC)___ Standards___ Spectra Quality___ Chromatography___ Data Completeness
This portion of the case consisted of five water samples which wereanalyzed according to CLP SOW 02/88 (Rev. 05/89) for TCL volatiletarget compounds on 12-06,07-89.
Sample BZ-1-0-1, BZ-l-0-2 and BZ-1-0-5 required 100-fold dilutionsdue to the high levels of chlorobenzene. The diluted result is tobe used for this compound only, since it exceeded the calibrationrange. All other results come from the original analysis.
The following samples had surrogate recoveries exceed the EPA CLPQC limits.
Sample Surrogate
BZ-1-0-1 1,2-DichloroethaneBZ-l-0-2 1,2-DichloroethaneBZ-1-0-2DL TolueneBZ-1-0-5DL 1,2-DichloroethaneBZ-1-0-5MS 1,2-DichloroethaneBZ-1-0-5MSD 1,2-Dichloroethane
All positive results and quantitation limits for these samples areconsidered estimated and are flagged "J" and "UJ".
4-Methyl-2-pentanone had response factors less than 0.05 in theinitial and continuing calibrations. Also, the 2-butanone responsefactor in the continuing calibration (12-07-89) was less than the0.05 QC limit. The associated quantitation limits for thesecompounds are rejected and flagged "R" in the data summary.
SR303!
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASES 8912L698,749,768PAGE 3 OF 7
The laboratory blanks contain common contaminants methylenechloride and acetone at levels less than 3X the CRQL. Allassociated positive results that are less than 10 times the blanklevel, have the quantitation limits adjusted to the reported valueand are flagged "U". The positive results for sample BZ-l-O-l andBZ-l-0-2 are above 10X the blank level, and are considered truevalues.
Several compounds had %RSD and %D for initial and continuingcalibrations exceed the 30 and 25% EPA QC limits. All associatedpositive results and guantitation limits are qualified estimated,"J" and "UJ".
The matrix spike/spike duplicate recoveries for benzene andchlorobenzene are reported at 0% recovery. The sample and its QCanalyses have high levels of these target compounds; therefore thecalculations of the spike recoveries were affected by these highconcentrations.
The %relative abundances for the tune on 12-06-89 at 09:06 werecorrected due to differences in values between the Form V and massspectra/mass list. The corrected Form V is resubmitted. All tunecriteria was met.
Several unknown compounds were detected in most samples asTentatively Identified Compounds (Tie's).
RR303101
III
EVALUATION BY FRACTION
II. Base/Neutral/Acids
___ Holding Time___ Extraction Timex Surrogate Recoveryx Blank
_JS_ MS/MSD___ GC/MS Tuningx Initial Calibrationx Continuing Calibration___ Compound ID (HSL, TIC)x Standards___ Spectra Quality___ Chromatography___ Data Completeness
This portion of the case consisted of four water samples which wereanalyzed according to CLP SOW 02/88 (Rev. 05/89) for TCL and clientspecified semivolatile target compounds on 01-05,06,09,10-90.
Sample BZ-1-0-1, BZ-1-0-2 and BZ-1-0-5 required 500-fold dilutionsbecause they contained high levels of chlorobenzene targetcompounds. The diluted results will be used for only thosespecific compounds that were out of calibration range on theoriginal analysis. All surrogate recoveries were not able to beobtained due to the dilutions.
The internal standard areas for 1,4-dichlorobenzene, naphthaleneand acenaphthene were below control limits in samples BZ-1-0-1, BZ-1-0-2 and BZ-1-0-5. The sample results may be biased high;therefore, all associated positive results and quantitation limitsare qualified estimated and flagged "J" and "UJ".
The matrix spike/spike duplicate recoveries and %RPD for 1,4-Dichlorobenzene and 1,2,4-trichlorobenzene were outside the EPA CLPQC limits. The original sample and its associated QC samples hadhigh levels of these compounds, thus affecting the spike recoveryresults. No qualification has been applied.
Several compounds had %RSD and %D in the initial and continuingcalibrations exceed the 30 and 25% EPA QC limits. The only sampleaffected is BZ-1-0-3, since the other samples have already beenqualified due to internal standard outliers. For sample BZ-1-0-3all associated quantitation limits are qualified estimated and areflagged KUJ" in the data summary.
flR303IQ2
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASES 89121,698,749,768PAGE 5 OF 7
The nitrobenzene surrogate recovery for sample B2-1-0-1 and BZ-1-0-2 exceeded the EPA CLP QC limits. However, EPA CLP surrogatecriteria were met (ie., no more than one outlier per fraction, andno recoveries less than 10%) .
The laboratory blank contains target compound 1,4-dichlorobenzeneat a level less than the CRQL. Samples BZ-l-O-l, BZ-1-0-2 and BZ-1-0-5 contain very high levels of this compound; therefore, noqualification is applied relative to this blank contamination. Thesample results were above 10X the blank level, and are consideredtrue values.
The 4-chloro-3-methylphenol spectra for sample BZ-1-0-1 and thespectra for TIC RT=10.5 for sample BZ-1-0-5 were missing from theoriginal data package. These have been submitted with this report.
The following nine client specified compounds were library searchedand several were detected in these samples: aniline, n-nitroso-diphenylamine, benzidine, 1,2,3-trichlorobenzene, 1,3,5-trichloro-benzene, 1,2,4,5-tetrachlorobenzene, 1,2,3,4-tetrachlorobenzene,pentachlorobenzene, and l-chloro-3-nitrobenzene.
Many unknown and chlorobenzene compounds were detected in thesesamples as Tentatively Identified Compounds (Tic's).
flR303i03
III
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASES 8912L698,749,768PAGE 6 OF 7
EVALUATION BY FRACTION
III* Pesticides/PCB
Holding TimeExtraction TimeSurrogate RecoveryMS/MSDBlankLinearity CalibrationDDT/Endrin DegradationAnalytical SequenceDEC Retention Time ——Continuing CalibrationRetention Time Window
___ Standards___ Chromatography -___ HSL Compounds___ Data Completeness
This portion of the cases consisted of five water and three soilsample which were analyzed for TCL Pesticide/PCB target compoundson 01-11,12-90.
Positive results for pesticide/PCB target compounds were not foundin these samples.
The following samples required dilutions due to high levels of non-target compounds:
Sample Dilution Factor
B2-1-0-1 10*BZ-l-0-2 10BZ-1-0-3 5*SS-13-1-1 MS/MSD 5*SS-13-l-2 5*SS-13-l-5 5
* Surrogate recoveries were not able to be obtained due tointerference of the non-target compounds.
The gamma-BHC matrix spike/spike duplicate recoveries could not beobtained due to non-target compound interference. Also the matrixspike duplicate recovery for heptachlor (133%) exceeded the EPA CLPQC limit (130%). There is no impact on the data since thesecompounds were not detected in the samples. KkW
AR303I04
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASES 89121,698,749,768PAGE 7 OF 7
All blank spike recoveries were within EPA CLP QC limits.
The %D on the primary column analyzed on 01-12-90 for heptachlorepoxide, dieldrin, endosulfan II (IND A 01-12-90 at 06:46), aldrin,endrin (IND B 01-12-90 at 14:34), heptachlor epoxide, dieldrin,endosulfan II (IND A 01-12-90 at 16:13) and aldrin, 4,4'-DDE,endrin (IND B 01-12-90 at 16:46) exceeded the 15% required QClimit. These compounds were not detected in the samples;therefore, there is no impact to the data.
The endrin %D on the confirmation columns (IND A 01-12-90 at 16:49)and (IND B 01-12-90 at 16:49) exceeded the 20% QC limit. Also, theendrin retention times in (IND B 01-12-90 at 14:36) and (IND B01-12-90 at 16:49) exceeded the established retention time windowson the confirmation column. Endrin was not found in any samples;therefore, no qualification is applied.
fiR303!05
IMFORMMION HEOMPIKO . DMPA
All data were reviewed according to EPA CLP Functional Guidelinesfor Evaluating Organic Analyses. All data have been validated withregard to usability.
If you have any questions or comments on this data review, pleasecall Zohreh Hamid at (215)524-7360.
1. Glossary of Data Qualifier Codes.
2. Data Summary. This includes:
a) All positive results for the target analyteswith the qualifier codes, if applicable; and
b) All unusable detection limits (qualified "R") .
3 . Support Documentation includes details to support thestatements in this reports.
6R303I06
GLOSSARY OF DATA QUALIFIERS
COD1S RELATING TO IDENTIFICATION
(confidence concerning presence or absence of compounds)
XT - NOT DETECTED, SUBSTANTIALLY ABOVE THE LEVELREPORTED IN LABORATORY OR FIELD BLANKS.
UNRELIABLE RESULT* ANALYTE MAY OR MAY NOT BEPRESENT IN THE SAMPLE. SUPPORTING DATANECESSARY TO CONFIRM RESULT.
V « NEGATED COMPOUND WAS CONSIDERED AS NOTPRESENT IN THE SAMPLE,
{NO CODE) = CONFIRMED IDENTIFICATION
CODES RELATING TO OUAKTITATION
(can be used for both positive results and sample quantitationlimits)':
J * ANALYTE PRESENT. REPORTED VALUE MAY NOT BEACCURATE OR PRECISE.
« THE REPORTED QUANTITATION LIMITS AREQUALIFIED ESTIMATED.
OTHER CODES
Q NO ANALYTICAL RESULT.
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-- CALIBRATION - BRQMQFLUORQBBNZBNB <BFB)
Mamex BQV T* W««ton> Inc. Contract: 2267-09*02*0000
CAM Ho. i STAHDAJtD CHLORINE______
Lab File ID: AKC601 BFB Injection Data: 12/06/89
Instrument ID: HP-MSD_K BFB Injection Time: 906
Matrix:(soil/water) WATgR Levels(low/med) LOW Column:(pack/cap) CAP
a/e•>•.50759596173174175176177
'ION ABUNDANCE CRITERIA
15.0 - 40.0% of mass 9530.0 - 60.0% of mass 95Base peak, 100% relative abundance5.0 - 9.0% of mass 95Leas than 2.0% of mass 174Greater than 50.0% of mass 955.0 - -9.0% of mass 174Greater than 95.0% but less than 101.0% of mass 175.0 - 9.0% of mass 176
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1 % RELATIVEj ABUNDANCE
I ^ - f.7\ .sa-rff 6 3\ 100.0j 3<{tf b* t\ 0.0{ 0.0)1I B?<fT olp."3 y a| 5.0( .8*-S)l$\ j?*3\ 100.0)1
\ 4-J -7.£1-Value is % mass 174 2-Value is % mass 176
THIS TONS APPLIES TO THE FOLLOWING SAMPLES, MS, MSD, BLANKS, AND STANDARDS:
| CLIENTj SAMPLE NO.
01 1 VSTDSO02 | VBLKLVK016-HB103 | B2-1-0-104 | BZ-1-0-205 1 BZ-1-0-306 | BZ-1-0-407 1 BZ-1-0-5MS08] BZ-1-0-5HSD09 j 88-1-0-510 1HI12 j13 [
15 116117 113 119120|
| LABj SAMPLE ID
I VSTDSO1 89LVK016-KB1j 8912L698-001j 8912L698-002j 8912L698-003| 8912L698-004| 8912L698-005S| 8912L698-005T| 8912L698-0051III11I11111
LABFILE ID
AKC602AKC603.AKC609 .AKC610.AKC611.AKC612.AKC613.AKC614.AKC615.
DATEANALYZED
12/06/8912/06/8912/06/8912/06/8912/06/8912/06/8912/06/8912/06/8912/06/89
| TIME| ANALYZED
| 0933| 1111| 1511j 1636j 1709| 17421 1815j 1848| 19221111111I1I11
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page 1 of 1 FORM V VGA 1/87 Rev.
AR3Q31 16
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I STAHDARD CHLORINECASE 8912L768
This quality assurance review is based upon a review of the datagenerated from two water samples collected on 12-07-89 andanalyzed by Roy F. Weston Lionville Analytical Laboratory for TCLVolatile and Semivolatile target compounds.
The reported analytical results are presented as a summary of thedata in Section II. All of the analytical data were examined todetermine the usability of the analytical results and also todetermine contractual compliance relative to the analyticalrequirements and deliverables specified in EPA's ContractLaboratory Program (CLP) protocol. Qualifier codes have beenassigned next to the results so that the data user can quicklyassess the qualitative and/or quantitative reliability of anyresults.
Details of this quality assurance review are presented in thenarrative section of this report under each fraction. This reportwas prepared to provide a critical review of the laboratoryanalyses and reported analytical results.
INFORMATION REGARDING DATA
All data were reviewed according to CLP Functional Guidelines forEvaluating Organic Analyses. All data have been validated withregard to usability.
If you have any questions or comments on this data review, pleasecall Zohreh Hamid at (215)524-7360.
ATTACHMENTS
1. Attachment I - Glossary of Data Qualifier Codes.
2. Attachment II - Data Summary. This includes:
a) All positive results for the target analyteswith the qualifier codes, if applicable; and
b) All unusable detection limits (qualified "R") .
fiR303i2l
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8912L768PAGE 2 OF 3
EVALUATION BY FRACTION
I- Volatiles
Holding Time ' __Surrogate Recovery ~~MS/MSDBlankGC/MS TuningInitial CalibrationContinuing Calibration
___ Compound ID (HSL, TIC)___ Standards___ Spectra Quality___ Chromatography___ Data Completeness
This portion of the case consisted of two water samples which wereanalyzed according to CLP SOW 02/88 (Rev. 05/89) for TCL Volatiletarget compounds on 12-12,15-89.
Samples SS-16-0-3 and SS-16-0-4 had the toluene and 1,2 dichloro-ethane surrogate recoveries exceed the EPA QC limits. The sampleswere re-analyzed within holding time and there were no surrogateoutliers. Therefore, the re-analysis should be used as therepresentative results.
* -Several compounds had %RSD and %D in the initial and continuingcalibrations exceed the 30% and 25% EPA QC limits. All associatedquantitation limits are qualified estimated "UJ".
The matrix spike associated with prep batch 89LVB103 is sample SW-18-0-5 (8912L769-005). The QC samples were re-analyzed at a higherdilution due to surrogate outliers and high levels of .targetcompounds. The original spike/spike duplicate recoveries forchlorobenzene were below the EPA QC limits; however, this was thetarget compound that exceeded the calibration range. On the otherhand, the re-analysis spike recoveries for benzene exceeded the EPAQC limits. Neither set of QC samples are a good evaluation of thelong term precision and accuracy of the analytical method. Noqualification is applied on this basis alone.
SR303122
QA ORGANIC DATA REVIEWSTANDARD CHLORINECASE 8912L768PAGE 3 OF 3
EVALUATION BY FRACTION
II. Base/Neutral/Acids
Holding TimeExtraction TimeSurrogate RecoveryBlankMS/MSDGC/MS TuningInitial CalibrationContinuing CalibrationCompound ID (HSL, TIC)StandardsSpectra QualityChromatographyData Completeness
This portion of the case consisted of one water sample which wasanalyzed according to CLP SOW 02/88 (Rev. 05/89) for TCL Volatiletarget compounds on 01-06-90.
Positive target compounds were not found in this sample. Allsurrogate, blank spike, and internal standard area criteria aremet. Also, the laboratory blank was free of contamination.
Several compounds had %RSD and %D in the initial and continuingcalibrations exceed the 30% and 25% EPA CLP QC limits. Theassociated quantitation limits are qualified estimated and flagged"UJ" in the data summary.
A matrix spike/spike duplicate sample was not analyzed with thisbatch. The long term precision and accuracy of the analyticalmethod can be evaluated according to the blank spike recoveries.No qualification is applied on this basis alone.
The following nine client specified target compounds were librarysearched and none were detected in this sample:
aniline, n-nitrosodiphenylamine, benzidiner1,2,3-trichlorobenzene, 1,3,5-trichlorobenzene, •1,2,4,5-tetrachlorobenzene, 1,2,3,4-tetrachlorobenzene,pentachlorobenzene, and l-chloro-3-nitrobenzene
flR303i23