Question Your Data. Jim Hays EXPERIMENT:

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1 Question Your Data EXPERIMENT: A SCIENTIFIC PROCEDURE UNDERTAKEN TO MAKE A DISCOVERY, TEST A HYPOTHESIS OR DEMONSTRATE A KNOWN FACT. Jim Hays JHays@encolabs.com

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3 Laboratory Certification 3 INSTITUTE.ORG/CONTENT/ABDB.PHP

4 Outline Sample Receipt Confirmation Method Detection Limits and Reporting Limits Analyte Recovery Limits Interpreting a Level II report Quality Assurance / Quality Control

5 Sample Receipt Confirmation

6 What is an MDL? METHOD DETECTION LIMIT (MDL) are set such that the constituent concentration, when processed through the complete method, produces a signal with a 99% probability that it is different from the blank. MDLs are updated annually or any time there is a significant change in laboratory operations.

7 What is a PQL or MRL? PRACTICAL QUANTITATION LIMIT (PQL) 3 to 5 times the calculated MDL unless otherwise noted. Published PQLs may be set higher than experimentally determined PQLs to: 1) Avoid observed positive interferences from matrix effects or common reagent contaminants, or 2) For reporting convenience (i.e., to group common compounds with similar but slightly different experimentally determined PQLs).

8 Why the metric system? What is a part per million (ppm or mg/l)? One ounce in 32 tons gal or 84 ½ oz. in an Olympic sized pool

9 Why the Metric System What is a part per billion (ppb or ug/l)? One kernel of corn in a silo 45-feet high and 16- feet in diameter. One second of time in 32 years A thimble in an Olympic sized pool.

10 Why the metric system? What is a part per trillion (ppt or ng/l)? One Part Per Trillion A 6 inch leap on a journey to the sun

11 Interpreting Analytical Data ENVIRONMENTAL ANALYTICAL CHEMISTRY CHEMBOOK_INDEX.HTML

12 Laboratory Report Data Package Types Report/Package Sections Level I * Level II Level III Level IV Level V Cover page X X X X Project Narrative X X X X Sample Summary / Lab Chronicle X X X X Sample Detection Summary X X X X Analytical Results (CLP-Like form 1's) X X X X X QC Data (MS/MSD, LCS, and Blanks) X X X X Flags / Notes and Definitions X X X X Chain of Custody Records (COC) X X X X CLP-like QC summary forms X X X All raw instrument data X X Laboratory bench / prep sheets X X Laboratory standards tracking report X * Level I is no longer offered for landfill groundwater work. Notes: 1 - "CLP-like" - CLP forms comply with the EPA CLP program requirements and analytical methods. CLP methods follow the TAL/TCL analyte lists which do not include many of the Wet Chem and State specific methods. Also, SW-846 methods may include different (or not include) performance criteria found in CLP methods. Hence the CLP-like forms for non-clp projects.

13 Level II Analytical Report Cover page Narrative (as needed) Results Surrogate recoveries Blank results Laboratory Control Samples (LCS) Matrix Spike (MS) Matrix Spike Duplicate (MSD) Chain of Custody (COC)

14 Verifying Methods and Hold Times

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16 Flags / Notes and Definitions B: The analyte was detected in the associated method blank. D: The sample was analyzed at dilution. J: The reported value is between the laboratory Method Detection Limit (MDL) and the laboratory Method Reporting Limit (MRL). This value is considered an estimate. U: The analyte was analyzed for but not detected. E: The concentration indicated for this analyte is an estimated value above the calibration range of the instrument. This value is considered an estimate.

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18 Metals ICP Inductively Coupled Plasma ICP/MS - Inductively Coupled Plasma Mass Spectrometry. CVAA Cold Vapor Atomic Absorption

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20 Surrogates and how we use them in the lab Volatiles w % Recovery Limit of % 97% 93% 112% 41% (fail)

21 Gas Chromatography and Gas Chromatography Mass Spectra GC dual dissimilar column GC/MS single column

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23 Verify qualifiers definition. D = Dilution D = Detected, but RPD is >40% between results in dual column method.

24 Grassy Chromatogram

25 Nice Chromatogram

26 GC/MS Volatiles Auto-Sampler Instrument

27 Volatile Organic Compounds by GC/MS Analyte [CAS Number] Results Flag Units DF MDL PQL Batch Method Analyzed By Notes 1,1,1,2-Tetrachloroethane [ ]" 0.61 U ug/l L27007 EPA /27/13 14:47 Kat 1,1,1-Trichloroethane [ ]" 0.80 U ug/l L27007 EPA /27/13 14:47 kat 1,1,2,2-Tetrachloroethane [ ]" 0.54 U ug/l L27007 EPA /27/13 14:47 kat 1,1,2-Trichloroethane [ ]" 0.76 U ug/l L27007 EPA /27/13 14:47 kat 1,1-Dichloroethane [ ]" 0.62 U ug/l L27007 EPA /27/13 14:47 kat 1,1-Dichloroethene [ ]" 0.94 U ug/l L27007 EPA /27/13 14:47 kat 1,1-Dichloropropene [ ]" 0.74 U ug/l L27007 EPA /27/13 14:47 kat 1,2,3-Trichloropropane [ ]" 0.64 U ug/l L27007 EPA /27/13 14:47 kat 1,2,4-Trichlorobenzene [ ]" 0.70 U ug/l L27007 EPA /27/13 14:47 kat 1,2-Dichlorobenzene [ ]" 0.73 U ug/l L27007 EPA /27/13 14:47 kat 1,2-Dichloroethane [ ]" 0.63 U ug/l L27007 EPA /27/13 14:47 kat 1,2-Dichloropropane [ ]" 0.80 U ug/l L27007 EPA /27/13 14:47 kat 1,3-Dichlorobenzene [ ]" 0.77 U ug/l L27007 EPA /27/13 14:47 kat 1,3-Dichloropropane [ ]" 0.60 U ug/l L27007 EPA /27/13 14:47 kat 1,4-Dichlorobenzene [ ]A 1.7 ug/l L27007 EPA /27/13 14:47 kat Surrogates Results DF Spike %Rec %Rec Limits Batch Method Analyzed By Notes Lvl 4-8romofluorobenzene % L27007 EPA /27/13 14:47 kat Dibromofluoromethane % L27007 EPA /27/13 14:47 kat Toluene-d % L27007 EPA /27/13 14:47 kat

28 Semivolatile Organic Compounds by GC/MS Analyte [CAS Number] N-Nitroso-di-n-propylamine [ ]" Results 4.5 Flag U Units ug/l DF 1 MDL 4.5 PQL 10 Batch 3L23027 Method EPA 8270D Analyzed 12/31/13 17:19 By jfi Notes N-nitrosodiphenylamine / Diphenylamine [ / ]" U U ug/l ug/l L L23027 EPA 8270D EPA 8270D 12/31/13 17:19 12/31/13 17:19 jfi jfi N-Nitrosomethylethylamine [ ]" N-Nitrosopiperidine [ ]" 3.9 U ug/l L23027 EPA 8270D 12/31/13 17:19 jfi N-Nitrosopyrrolidine [ ]" 4.2 U ug/l L23027 EPA 8270D 12/31/13 17:19 jfi QM- 07 O,O,O-Triethyl phosphorothioate [ ]" o-toluidine [ ]" U U ug/l ug/l L L23027 EPA 8270D EPA 8270D 12/31/13 17:19 12/31/13 17:19 jfi jfi Parathion [ ]" 1.2 U ug/l L23027 EPA 8270D 12/31/13 17:19 jfi p-dimethylaminoazobenzene [ ]" 3.4 U ug/l L23027 EPA 8270D 12/31/13 17:19 jfi Pentachlorobenzene [ ]" 3.0 U ug/l L23027 EPA 8270D 12/31/13 17:19 jfi Pentachloronitrobenzene [ ]" 3.2 U ug/l L23027 EPA 8270D 12/31/13 17:19 jfi Surrogates Results DF Spike %Rec %Rec Limits Batch Method Analyzed By Notes Lvl 2,4,6-Tribromophenol % L23027 EPA 8270D 12/31/13 17:19 jfi 2-Fluorobiphenyl % L23027 EPA 8270D 12/31/13 17:19 jfi 2-Fluorophenol % L23027 EPA 8270D 12/31/13 17:19 jfi Nitrobenzene-d % L23027 EPA 8270D 12/31/13 17:19 jfi Phenol-d % L23027 EPA 8270D 12/31/13 17:19 jfi Terphenyl-d % L23027 EPA 8270D 12/31/13 17:19 jfi

29 Chlorinated Herbicides by GC Analyte [CAS Number] 2,4,5-T [ ]" Results 0.23 Flag U Units ug/l DF 1 MDL 0.23 PQL 0.50 Batch 3L23005 Method EPA 8151A Analyzed 12/26/13 16:00 By RGG Note s 2,4,5-TP (Silvex) [ ]" 0.20 U ug/l L23005 EPA 8151A 12/26/13 16:00 RGG QL-02 2,4-D [ ]" 0.16 U ug/l L23005 EPA 8151A 12/26/13 16:00 RGG Dinoseb [ ]" 0.32 U ug/l L23005 EPA 8151A 12/26/13 16:00 RGG QM- 07 Pentachlorophenol [ ]" 0.19 U ug/l L23005 EPA 8151A 12/26/13 16:00 RGG Surrogates Results DF Spike %Rec %Rec Batch Method Analyzed By Notes Lvl Limits 2,4-DCAA % L23005 EPA 8151A 12/26/13 16:00 RG G

30 Polychlorinated Biphenyls by GC Analyte [CAS Number] Results Flag Units DF MDL PQL Batch Method Analyzed By Notes PC8-1016/1242 [ / ]" 0.43 U ug/l L19010 EPA 8082A 12/20/13 15:28 MSZ PC [ ]" 0.37 U ug/l L19010 EPA 8082A 12/20/13 15:28 MSZ PC [ ]" 0.35 U ug/l L19010 EPA 8082A 12/20/13 15:28 MSZ PC [ ]" U ug/l L19010 EPA 8082A 12/20/13 15:28 MSZ PC [ ]" U ug/l L19010 EPA 8082A 12/20/13 15:28 MSZ PC [ ]" 0.45 U ug/l L19010 EPA 8082A 12/20/13 15:28 MSZ Surrogates Results DF Spike Lvl %Rec %Rec Limits Batch Method Analyzed By Notes 2,4,5,6-TCMX % L19010 EPA 8082A 12/20/13 15:28 MSZ Decachlorobiphenyl % L19010 EPA 8082A 12/20/13 15:28 MSZ PCB Aroclors are multi-component mixture of congeners. Many of the congeners are shared with the same Aroclor. TOTAL PCB s is not the sum of the Aroclor s, But the sum of the 19 primary congeners with a total of 209 available.

31 SW-846 Method 8082A Table 6

32 QA section of the report Blank results Laboratory Control Samples (LCS) Matrix Spike (MS) Matrix Spike Duplicate (MSD)

33 Quality Control Data Volatile Organic Compounds by GCMS Blank (3L19031-BLK1) Prepared: 12/19/ :46 Analyzed: 12/19/ :48 Analyte Batch 3L EPA 5030B_MS Result Flag PQL Units Spike Level Source Result orec orec Limits RPD RPD Limit Notes 1,1,1,2-Tetrachloroethane 0.17 U 1.0 ug/l 1,1,1-Trichloroethane 0.12 U 1.0 ug/l 1,1,2,2-Tetrachloroethane 0.28 U 1.0 ug/l 1,1,2-Trichloroethane 0.14 U 1.0 ug/l 1,1-Dichloroethane 0.13 U 1.0 ug/l 1,1-Dichloroethene 0.21 U 1.0 ug/l 1,2,3-Trichloropropane 0.23 U 1.0 ug/l 1,2-Dichlorobenzene 0.19 U 1.0 ug/l 1,2-Dichloroethane 0.21 U 1.0 ug/l 1,2-Dichloropropane 0.10 U 1.0 ug/l 1,4-Dichlorobenzene 0.19 U 1.0 ug/l 2-8utanone 1.3 U 5.0 ug/l 2-Hexanone 0.88 U 5.0 ug/l 4-Methyl-2-pentanone 1.1 U 5.0 ug/l Acetone 1.2 U 5.0 ug/l Acrylonitrile 3.5 U 10 ug/l 8enzene 0.15 U 1.0 ug/l 8romochloromethane 0.48 U 1.0 ug/l 8romodichloromethane 0.17 U 1.0 ug/l 8romoform 0.22 U 1.0 ug/l 8romomethane 0.14 U 1.0 ug/l

34 Quality Control Data Volatile Organic Compounds by GCMS Laboratory Control Sample (LCS) Batch 3L EPA 5030B_MS - Continued LCS (3L19031-BS1) Prepared: 12/19/ :46 Analyzed: 12/19/ :18 Analyte Result Flag PQL Units Spike Level %REC %REC Limits RPD RPD Limit Notes 1,1-Dichloroethene ug/l enzene ug/l Chlorobenzene ug/l Toluene ug/l Trichloroethene ug/l romofluorobenzene 51 ug/l Dibromofluoromethane 45 ug/l Toluene-d8 50 ug/l

35 Matrix Spike/Matrix Spike Duplicate Matrix Spike (3L19019-MS1) Source: C Analyte Result Flag PQL Units Spike Level Source Result %REC % REC Limits Arsenic ug/l U arium ug/l eryllium ug/l Cadmium ug/l U Chromium ug/l U Copper ug/l U Lead ug/l Nickel ug/l Tin ug/l U Vanadium ug/l Zinc ug/l Matrix Spike Dup (3L19019-MSD1) RPD RPD Limit Source: C Analyte Result Flag PQL Units Spike Level Source Result orec % REC Limits RPD RDP Limit Arsenic ug/l U arium ug/l eryllium ug/l Cadmium ug/l U Chromium ug/l U Copper ug/l U Lead ug/l Nickel ug/l Tin ug/l U Vanadium ug/l Zinc ug/l

36 Matrix Spike/Matrix Spike Duplicate Matrix Spike (3L19019-MS1) Source: C Analyte Result Flag PQL Units Spike Level Source Result %REC % REC Limits Arsenic ug/l U arium ug/l eryllium ug/l Cadmium ug/l U Chromium ug/l U Copper ug/l U Lead ug/l Nickel ug/l Tin ug/l U Vanadium ug/l Zinc ug/l Matrix Spike Dup (3L19019-MSD1) RPD RPD Limit Source: C Analyte Result Flag PQL Units Spike Level Source Result orec % REC Limits RPD RDP Limit Arsenic ug/l U arium ug/l eryllium ug/l Cadmium ug/l U Chromium ug/l U Copper ug/l U Lead ug/l Nickel ug/l Tin ug/l U Vanadium ug/l Zinc ug/l

37 Matrix Spike/Matrix Spike Duplicate Matrix Spike (3L19019-MS1) Source: C Analyte Result Flag PQL Units Spike Level Source Result %REC % REC Limits Arsenic ug/l U arium ug/l eryllium ug/l Cadmium ug/l U Chromium ug/l U Copper ug/l U Lead ug/l Nickel ug/l Tin ug/l U Vanadium ug/l Zinc ug/l Matrix Spike Dup (3L19019-MSD1) RPD RPD Limit Source: C Analyte Result Flag PQL Units Spike Level Source Result orec % REC Limits RPD RDP Limit Arsenic ug/l U arium ug/l eryllium ug/l Cadmium ug/l U Chromium ug/l U Copper ug/l U Lead ug/l Nickel ug/l Tin ug/l U Vanadium ug/l Zinc ug/l

38 Matrix Spike/Matrix Spike Duplicate Matrix Spike (3L19019-MS1) Source: C Analyte Result Flag PQL Units Spike Level Source Result %REC % REC Limits Arsenic ug/l U arium ug/l eryllium ug/l Cadmium ug/l U Chromium ug/l U Copper ug/l U Lead ug/l Nickel ug/l Tin ug/l U Vanadium ug/l Zinc ug/l Matrix Spike Dup (3L19019-MSD1) RPD RPD Limit Source: C Analyte Result Flag PQL Units Spike Level Source Result orec % REC Limits RPD RDP Limit Arsenic ug/l U arium ug/l eryllium ug/l Cadmium ug/l U Chromium ug/l U Copper ug/l U Lead ug/l Nickel ug/l Tin ug/l U Vanadium ug/l Zinc ug/l

39 SUMMARY The Chain of Custody is a legal document. Treat it as such. Verify your project is logged in properly. Look at your data as soon as you receive it. Make sure holding times were met. Verify QA/QC and if there was an issue it is pointed out by the lab in the narrative. Any project could go to court. Make sure your data is defensible.

40 Jim Hays ENCO LABS CARY, NC / ORLANDO, FL JACKSONVILLE, FL (919) CELL JHAYS@ENCOLABS.COM