Total Extractable Petroleum Hydrocarbons (Diesel) Alamos National Labs/TA 03... · Case Narrative . New Mexico ... Work Order Number: 1111251 . 1. This report consists of 1 water

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03 LAfvl G\-'"olAl1. cJ~t(" r-~ ENTERED R- b I /}n IIil1 Mil- (~Pit SC,w.rl-ef. il/17/11

TA-S ()\ol-1z:.."'.da...ct Cc-..y ~

Total Extractable Petroleum Hydrocarbons

(Diesel)

Case Narrative

New Mexico Environment Department 08 LMW08 - 813-11.15.11 (HWB Proj)PAR-all-files

Work Order Number: 1111251

1. This report consists of 1 water sample and 1 solid sample. The samples were received cool and intact by ALS on 11/17/2011.

2. The water sample was extracted by adding hexane to _the water sample and shaking the resulting two phase solution according to SOP 603 Revision 12, which was developed at ALS. The hydrocarbons partition into the hexane layer, which is then removed for analysis.

The solid sample was extracted by adding a methanollwater solution to the soil followed by hexane according to SOP 603 Revision 12, which was developed at ALS. This mixture is shaken and the hexane portion of the two-phase solution is removed for analysis.

3. The extracts were then analyzed using GC with a capillary column and a flame ionization detector (FlO) according to SOP 406 Revision 15 generally based on SW-846 Method 8000B and Method 8015B. The procedures are based on this general method because SW-846 does not have a specific method for total extractable petroleum hydrocarbons (TEPH) or diesel range organics. The only true modification from this method is that TEPH is a multicomponent mixture and is quantitated by summing the entire range, rather than individual peaks. All positive results were quantitated using the responses from the initial calibration curve using the external standard technique. Also, a confirmation column is not used, because the analyte is a multicomponent mixture and the specific carbon range of the peaks detected is specified on the individual sample reporting forms.

4. All initial and continuing calibration criteria were met.

5. The method blanks associated with this project were below the MOL for diesel range organics.

6. All laboratory control sample and laboratory control sample duplicate recoveries and RPOs were within the acceptance criteria.

35029 1 of 14

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7. Per method requirements, matrix QC was performed for this analysis. Since a sample from this order number was not the selected quality control (QC) sample, matrix specffic QC results are not included in this report.

8. All samples were extracted and analyz.ed within the established holding time.

9. A surrogate recovery could not be reported for sample -3 due to the dilution needed to bring the target analyte into the linear range of the Instrument. All other surrogate recoveries were within the acceptance criteria.

10. Sample -3 was analyzed at a dilution in order to bring the target analyte within the calibration range of the instrument. The reporting limits have been adjusted accordingly.

11. Manual integrations are performed when needed to provide consistent and defensible data following the guidelines in SOP 939 Revision 4.

The data contained in the following report have been reviewed and approved by the personnel listed below. In addition, ALS certifies that the analyses reported herein are true, complete and correct within the limits of the methods employed.

Mindy No . Date Organics Primary Data Reviewer

Organics Final Data Reviewer Date

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http:analyz.ed

ALS Data Qualifier Flags Fuels

G: This flag indicates that a pattern resembling gasoline was detected in this sample.

D: This flag indicates that a pattern resembling diesel was detected in this sample.

M: This flag indicates that a pattern resembling motor oil was detected in this sample.

c: This flag indicates that a pattern resembling crude oil was detected in this sample.

4: This flag indicates that a pattern resembling JP-4 was detected in this sample.

5: This flag indicates that a pattern resembling JP-5 was detected in this sample.

H: This flag indicates that the fuel pattern was in the heavier end of the retention time window for the analyte of interest.

L: This flag indicates that the fuel pattern was in the lighter end of the retention time window for the analyte of interest.

Z: This flag indicates that a significant fraction of the reported result did not resemble the patterns of any of the following petroleum hydrocarbon products: gasoline JP-8 diesel mineral spirits motor oil Stoddard solvent bunker C

Multiple flags may be used to indicate the presence of more than one product or component.

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ALS Data Qualifier Flags Chromatography and Mass Spectrometry

U or NO: This flag indicates that the compound was analyzed for but not detected.

J: This flag indicates an estimated value. This flag is used as follows: (1) when estimating a concentration for tentatively identified compounds (TICs) where a 1:1 response is assumed; (2) when the mass spectral and retention time data indicate the presence of a compound that meets the volatile and semivolatile GC/MS identification criteria, and the result is less than the reporting limit (RL) but greater than the method detection limit (MOL); (3) when the data indicate the presence of a compound that meets the identification criteria, and the result is less than the RL but greater than the MOL; and (4) the reported value is estimated.

B: This flag is used when the analyte is detected in the associated method blank as well as in the sample. It indicates probable blank contamination and warns the data user. This flag shall be used for a tentatively identified compound (TIC) as well as for a positively identified target compound.

E: This flag identifies compounds whose concentration exceeds the upper level of the calibration range.

A: This flag indicates that a tentatively identified compound is a suspected aldol-condensation product.

X: This flag indicates that the analyte was diluted below an accurate quantitation level.

This flag indicates that a spike recovery is outside the control criteria.

+: This flag indicates that the relative percent difference (RPO) exceeds the control criteria.

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ALS Environmental -- Fe Sample Number(s) Cross-Reference Table

OrderNum: 1111251 Client Name: New lVIexico Environment Department OB

Client Project Name: LMW08 Client Project Number: 813-11.15.11 (HWB Proj)PAR-all-files

Client PO Number: 10-667-00-13453

Client Sample Number

Lab Sample Number

cac Number Matrix Date Collected

Time Collected

R-61 Sc 1-11-15-VOC 1111251-1 WA -rER 15-Nov-11 9:40 R-61 Sc 1-11-15-SVOC 1111251-2 WATER 15-Nov-11 9:40

SWR61 PADBASIN 1111251-3 SOLID 15-Nov-11 10:37

Page 1 of 1 ALS Environmental -- Fe Date Printed: Thursday, December 08, 2011 LlMS Version: 6.545

5 of 14

http:813-11.15.11

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COM)lT10I\; OF SAM PL UPON RECEIPT FORiVl

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Docs this project require: any special handling in addition to stand:mi Paragon procedurc:"") YES

11 Were all placed in the proper containers for the analyses': ' YES NO _... , ,- ---, ------~,---- , .. -,- - " Arc all sampl-=_s_vi_it~~~~~~ing times for the rcq,--u_es_t_e_d ____~__~_____~_~ _,.~__~...~t _~,:-(CJ,)____:. .. s' I.' Were all sample containers received intact? (not broken or leaking, etc) ~"

14 Are all samples requiring 00 hcadspace (YOe, GRO, RSK/MEE, Rx CN/S, radon) 8 NI:'\ YES NO

hcadspacc frec') Size of bubble: < green pca > green pca

I' Do perchlorate LCMS-MS samples have hcadspacc: (at least 1."3 of container required) YES NOB 16 Were samples checked for and free from tbe presence of residual chlorine?

1 A,-,piical:lc when Pyl Ita, i:]djc:l!~d samples lire from a chionnared water ,(lllrcc: note ir iicld prcscrc'atiol1 '(J-:S NOWJlh sodium lhl()~ldj;lt" \\a, not ;)h,crv;:d.)

- Were the samples shipped on ice?

\Verc cooler temperatures measured at O.I-6.0"C') IR gun used*: #2

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Background ~tR'hr reading; lJ I Were eXlernal ~R.hr readings" 1\", [l1llC~ background and wltbn DOT ;lc;;cplancc CT;lcriu') YES, NO! NA (11'110, ,cc: Fonll nOH"

Additional Infurmation: PRovlDr DETAILS BELOW FOR ... >":0 RfSPO)iSE TO A;\'Y OL'ESno:-.: ABOVE. EXCEPT": A:\()" 16,

Arc custody seals on shipping containers intact'!

Are Custody seals on sample containers intuct"

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4 Is there a COC (Chain-of-Custod~') present or other representative documents?

5 Arc the COC and bottle labels complete and legible'?

. Is the cac in agreement with samplcs received? (IDs. dates. times. no of samples, no. of containers. malnx, requested analyses, etc.)

\,Vere airbills / shipping documents present and/or removable?

, Arc all aqueous sampks n.'quiring preservation preserved correctly? (excluding volatiles)

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Diesel Range Organics Method SW8015MB

Method Blank

Lab Name: ALS Environmental .. FC


Client Name: New Mexico Environment Department OB

ClientProject 10: LMW08 813-11.15.11(HWB Proj)PAR-all-files

Lab 10: EXl11122-1MB Sample Matrix: WATER

% Moisture: N/A Prep Batch: EX111122-1

QCBatchlD: EX111122-1-1

Sample Aliquot:

Final Volume:

160 ml

4 ml Date Collected: N/A Run 10: HCD111122-3A Result Units: MG/L Date Extracted: 22-Nov-11 Cleanup: NONE Clean OF: 1 Date Analyzed: 23-Nov-11 Basis: N/A

File Name: F3F41436

CASNO Target Analyte OF Result Reporting MOL Result EPA Umit Qualifier Qualifier

68334-30-5 Diesel Range Organics 1 0.5 0.5 0.15 U

Surrogate Recovery

CASNO Surrogate Analyte Result Flag Spike Amount

Percent Recovery

Control Limits

84-15-1 0-TERPHENYL 1.07 1.25 86 57 - 132

Data Package ID: HCD1111251-1

Date Printed: Thursday, December 08, 2011 ALS Environmental -- FC Page 1 of 2 LlMS Version: 6.545

90f14


Sample Results

Lab Name: ALS Environmental FC



ClientProject 10: LMW08 813-11.15,11(HWB Proj)PAR-all-files

Field 10: R-61 Sc 1-11-15-SVOC Sample Matrix: WATER Prep Batch: EX111122-1 Sample Aliquot: 160ml

Lab 10: 1111251-2 0/0 Moisture: N/A

Date Collected: 15-Noy-11

QCBatchIO: EX111122-H

Run 10: HCD111122-3A

Final Volume:

Result Units: MGIL

4ml

Date Extracted: 22-Nov-11 Cleanup: NONE Clean OF: 1

Analysis ReqCode: 163 Date Analyzed: 23-NoY-11 Basis: As Received

Prep Method: METHOD File Name:F3F41446

CASNO Target Analyte Dilution Result Reporting MOL Result EPA Factor Limit Qualifier Qualifier

68334-30-5 Diesel Range Organics 1 0.5 0,5 0.15 U

Surrogate Recovery


Percent Recovery

Control Limits

84-15-1 O TERPHENYL 1 1.25 80 57 - 132


Date Printed: Thursday, December 08, 2011 ALS Environmental -- FC Page 1 of 2 LlMS Version: 6.545

10 of 14


Method Blank




ClientProject 10: LMW08 813-11.15.11(HWB Proj)PAR-all-files

Lab 10: EX111128-8MB Sample Matrix: SOLID


QC8atchlD: EX111128-8-1

Sample Aliquot:

Final Volume:

20 9

5 ml Date Collected: N/A Run 10: HCD111201-3A Result Units: MG/KG Date Extracted: 28-Nov-11 Cleanup: NONE Clean OF: 1 Date Analyzed: 02-Dec-11 Basis:N/A

File Name: F3F41481

CASNO Target Analyte DF Result Reporting MDL Result EPA Limit Qualifier Qualifier

68334-30-5 Diesel Range Organics 1 5 5 1.5 U

Surrogate Recovery


Percent Recovery

Control Limits

84-15-1 O-TERPHENYL 8.59 12.5 69 47 - 142

Data Package 10: HCD1111251-1

Date Printed: Thursday, December 08, 2011 ALS Environmental -- Fe Page 2 of 2 UMS Version: 6,545

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Sample Res~lts




ClientProject 10: LMW08 813-11.15.11(HWB ProilPAR-all-files

Field 10: SWR61 PADBASIN Sample Matrix: SOLID Prep Batch: EX111128-8 Sample Aliquot: 5.04g

Lab 10: 1111251-3 % Moisture: N/A

Oate Collected: 15-Nov-11 QCBatchIO: EX111128-8-1

Run 10: HCD111201-3A Final Volume: 5ml

Result Units: MG/KG Date Extracted: 28-Nov-11 Cleanup: NONE Clean OF: 1

Analysis ReqCode: 163 Oate Analyzed: 02-Dec-11

Prep Method: METHOD Basis: As Received

File Name:F3F41484

CASNO Target Analyte Dilution Factor

Result Reporting Limit

MOL Result Qualifier

EPA Qualifier

68334-30-5 Diesel Range Orgamcs 20 2900 400 120 Z,H

Surrogate Recovery


Percent Recovery

Control Limits

84-15-1 0-TERPHENYL X 49.6 47 - 142

The chromatogram for Diesel Range Organics indicates the presence of hydrocarbons in the range of C8 C40+.

Data Package ID: HCD11112S1-1

Date Printed: Thursday, December 08, 2011 ALS Environmental -- FC Page 2 of2 UMS Version: 6.545

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Laboratory Control Sample and Laboratory Control Sample Duplicate




ClientProject 10: LMW08 81311,15,11(HWB Proj)PAR-all-files

Lab 10: EX111122-1LCS

Sample Matrix: WATER


QCBatchlO: EX111122-1-1

Sample Aliquot:

Final Volume:

160 ml

4 ml Date Collected: N/A Run 10: HCD111122-3A Result Units: MG/L Date Extracted: 11/22/2011 Cleanup: NONE Clean OF: 1 Date Analyzed: 11/23/2011 Basis: N/A

Prep Method: METHOD File Name: F3F41437

CASNO Target Analyte Spike Added

LCS Result

Reporting Limit

Result Qualifier

LCS% Rec.

Control Limits

68334-30-5 Diesel Range Organics 5 4.75 0,5 95 36 150%

Lab 10: EXl11122-1LCSD Sample Matnx:WATER

% Moisture: N/A Prep Batch: EXl11122-1

QCBatchlD: EXl11122-H

Sample Aliquot:

Final Volume:

160 ml

4 ml

Date Collected: N/A Run 10: HCD111122-3A Result Units: MG/L Date Extracted: 11/2212011 Cleanup: NONE Clean OF: 1 Date Analyzed: 11/2312011 Basis: N/A

Prep Method: METHOD File Name: F3F41438


LCSD Result

Reporting Limit

Result Qualifier

LCSD % Rec.

RPD Limit

RPD

68334-30-5 Diesel Range Organics 5 4,8 0,5 96 20 1

Surrogate Recovery LCS/LCSD


LCS% Rec.

LCS Flag

LCSD% Rec.

LCSD Flag

Control Limits

84-15-1 0-TERPHENYL 1.25 91 92 57 132


Date Printed: Thursday, December 08,2011 ALS Environmental -- Fe Page 1 of 2 LlMS VersIon 6,545

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Laboratory Control Sample and Laboratory Control Sample Duplicate

Lab Name: ALS Environmental _. fC



ClientProject 10: LMW08 813-11. 15.11(HWB ProDPAR-all-files .;

Lab 10: EX111128-8LCS Sample Matrix: SOLID

% Moisture: N/A Prep Batch: EX111128-8 QCBatchlO: EX111128-8-1

Sample Aliquot: final Volume:

20 9 5 ml

Date Collected: N/A Run 10: HCD111201-3A Result Units: MG1KG Date Extracted: 11128/2011 Cleanup: NONE Clean Of: 1 Date Analyzed: 12/02/2011 Basis: N/A

Prep Method: METHOD file Name: F3F41482

CASNO Target Analyte Spike

68334-30-5 Diesel Range Organics

Added

50

LCS Result

Reporting Result Limit Qualifier

50.9 5

LCS% Control Ree. Limits

102 43 -139%

Lab 10: EX111128-8LCSD Sample Matrix: SOLID

% Moisture: N1A Prep Batch: EX111128-8 QCBatchlO: EX111128-8-1

Sample Aliquot: final Volume:

20 9 5 ml

Date Collected: N1A Run 10: HCD111201-3A Result Units: MG1KG Date Extracted: 11/28/2011 Cleanup: NONE Clean Of: 1 Oate Analyzed: 1210212011 Basis: N/A

Prep Method: METHOD file Name: F3F41483


LCSD Result

Reporting Limit

Result Qualifier

LCSD "10 Ree.

RPD Limit

RPD

68334-30-5 Diesel Range Organics 50 52.5 5 105 20 3

Surrogate Recovery LCS/LCSD


LCS% Ree.

LCS Flag

LCSD% Ree.

LCSD Flag

Control Limits

84-15-1 0-TERPHENYL 12.5 66 68 47 - 142

Data Package 10: HCD11112S1-1

Date Printed: Thursday, December OB, 2011 ALS Environmental- Fe Page 2 of2 LIMS Version: 6.545

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Quantitation Report

Data File C:\HPCHEM\5\DATA\120J,201J.\F3F41484.D Vial: 16 Acq On 02 Dec 11 07:44 AM Operator: jfn Sample 1111251- 3 20x lnst FUELS 3 Mise solidi 50uL!lmL FV Multiplr: 1.00 Quant Dec 2 20:38 19111

Method C:\HPCHBM\5\MBTHODS\0111B11A.M tle B01SBrr,od , CALuft

Last Update Fri Dec 02 20:33:35 2011

Response via Multiple Level Calibration

Volume Inj. 2uL

Signal Phase DB 5.625, 20m x O.25mm x O.5~m

Signal Info FID

~ance

I 9000 I

8000_

28

7 000 _

- i 6000

5000

4000

3000

2000

1000 \~. ~~------------------~

-->0.00

F3F41484.D D111811A.M Dec 02 20:38:20 2011 Page 2

GC/MS Semivolatiles

Case Narrative

New Mexico Environment Department OB

LMW08 - 813-11.15.11 (HWB ProDPAR-all-files


1 . This report consists of 1 water sample and 1 solid sample. These samples were received cool and intact by ALS on 11/17/11.

2. These samples were prepared and analyzed according to SW-846, 3rd Edition procedures.

The water sample was extracted using continuous liquid-liquid extractors, according to SW-846 Method 3520C utilizing SOP 617 Revision 14.

The solid sample was extracted using soxhlet procedures according to SW-846 Method 3540C utilizing SOP 625 Revision 12. This sample could only be brought to a final volume of 7 ml due to matrix issues, reporting limits have been adjusted to reflect this issue.

3. The extracts were analyzed using GC/MS with a OB-5MS capillary column according to SOP 506 Revision 19 based on SW-846 Method 82700. All positive results were quantitated against the initial calibration standards using the internal standard technique. The identification of positive results was achieved by a comparison of the retention time and mass spectrum of the sample versus the daily calibration standard.

4. All initial calibration criteria were met. If average response factors were used in the initial calibration, %RSO was :;;20%. If linear or higher order regression calibrations were used in the initial calibration, the coefficient of determination (~) ~0.99.

5. All initial calibration standards are verified by comparing a second source standard initial calibration verification (ICV) against the calibration curve. All target compounds in the second source verification had a %0 :530%.

6. All compounds in each of the daily (continuing) calibration verifications were within 20%0 with the exceptions of n-nitrosopyrrolidine, n-nitrosodi-n-butylamine and atrazine which were high on 12/01/11 and dinoseb which was low on 12101/11. None of these compounds were detected in the associated samples.

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http:813-11.15.11

7. All method blank criteria were met.

8. All laboratory control sample and laboratory control sample duplicate criteria were met with the following exception:

Spiked Compound QCSample Direction Benzidine EX111121-4LCS/LCSO &

EX111128-4LCS/LCSO Low

Benzidine is subject to oxidative losses during solvent concentration. The chromatographic behavior is non-reproducible and poor.

9. Since a sample from this order number was not the selected quality control (QC) sample, matrix specific QC results are not included in this report.

10. The samples were extracted and analyzed within the established holding times.

11. All surrogate recoveries were within acceptance limits with the following exceptions:

Surrogate Sample Direction 2,4,6-Tribromophenol 1111251-2 & High

EX111121-4LCS/LCSO

Because of the number of surrogates used by this method, the laboratory allows for samples to have one acid and/or one base/neutral surrogate outside limits if the remaining surrogates suggest the problem is matrix related and that there were no problems with the laboratories performance during the extraction and analysis.

12. All internal standard recoveries were within acceptance criteria with the following exceptions:

Internal Standard Sample Direction Phenanthrene-01Q 1111251-3 Low

Chrysene-012 1111251-3 Low

Re-analysis of the sample at dilution confirmed the original result. This suggests that the outliers were due to matrix effects. No further action was taken.

13. Due to matrix effects, a smaller initial aliquot of samples 1111251-3 was used. The final volume of this sample was 7ml, resulting in elevated reporting limits.

14. Manual integrations are performed when needed to provide consistent and defensible data following the guidelines in SOP 939 Revision 4.

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The data contained in the following report have been reviewed and approved by the personnel listed below. In addition, ALS certifies that the analyses reported herein are true, complete and correct within the limits of the methods employed.

~~Emily Helli son Date Organics rimary Data Reviewer

D~ \~,1J.?tl Date

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ALS Data Qualifier Flags Chromatography and Mass Spectrometry

U or NO: This flag indicates that the compound was analyzed for but not detected.

J: This flag indicates an estimated value. This flag is used as follows: (1) when estimating a concentration for tentatively identified compounds (TICs) where a 1:1 response is assumed; (2) when the mass spectral and retention time data indicate the presence of a compound that meets the volatile and semivolatile GC/MS identification criteria, and the result is less than the reporting limit (RL) but greater than the method detection limit (MOL); (3) when the retention time data indicate the presence of a compound that meets the GC identification criteria, and the result is less than the RL but greater than the MOL; and (4) the reported value is estimated.

B: This flag is used when the analyte is detected in the associated method blank as well as in the sample. It indicates probable blank contamination and warns the data user. This flag shall be used for a tentatively identified compound (TIC) as well as for a positively identified target compound.

E: This flag identifies compounds whose concentration exceeds the upper level of the calibration range.

A: This flag indicates that a tentatively identified compound is a suspected aldol-condensation product.

X: This flag indicates that the analyte was diluted below an accurate quantitation level.

*. This flag indicates that a spike recovery is equal to or outside the control criteria used.

+: This flag indicates that the relative percent difference (RPO) equals or exceeds the control criteria.

4 of 42

ALS Environmental -- Fe Sample Number(s) Cross-Reference Table

OrderNum: 1111251 Client Name: New Mexico Environment Department OB

Client Project Name: LMW08 Client Project Number: 813-11.15.11 (HWB ProDPAR-all-files

Client PO Number: 10-667-00-13453

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Total Extractable Petroleum Hydrocarbons (Diesel) Alamos National Labs/TA 03... · Case Narrative . New Mexico ... Work Order Number: 1111251 . 1. This report consists of 1 water