Sample RM Analytical Report ( B) HPLC/UV Analysis Acetaldehyde, Acrolein, Crotonaldehyde, Formaldehyde

Transcription

1 For the benefit of VaporFi, Inc. Sample RM Analytical Report ( B) HPLC/UV Analysis Acetaldehyde, Acrolein, Crotonaldehyde, Formaldehyde GC/MS/MS Analysis 1-Aminonaphthalene, 2-Aminonaphthalene, 4-Aminobiphenyl Enthalpy Analytical, Inc. Phone: (919) / Fax: (919) / Capitola Drive Durham, NC

2 I certify that to the best of my knowledge all analytical data presented in this report: Have been checked for completeness Are accurate, error-free, and legible Have been conducted in accordance with approved protocol, and that all deviations and analytical problems are summarized in the appropriate narrative(s) This analytical report was prepared in Portable Document Format (.PDF) and contains 97 pages. Report Issued: 09/16/2014 EA# B Page 2 of 97

3 Summary of Results EA# B Page 3 of 97

4 Report for: For the benefit of VaporFi, Inc. Project Code: Client Project: RM02 & HPHC Testing Project Start Date: 08/07/2014 Sample Type: eliquid Analysis Method: ENT301 Enthalpy Code Client Code Dilution Factor Acetaldehyde (ug/ml) Acrolein (ug/ml) Crotonaldehyd e (ug/ml) Formaldehyde (ug/ml) RM < 1.07 ND < 1.09 ND 10.2 ND: Not Detected; analytes not detected above the MDL Compound / Dilution MS Catch Spike Amnt Native Amnt Recovery Sample ID Factor (ug) (ug) (ug) % Acetaldehyde MS % Acrolein MS % Crotonaldehyde MS % Formaldehyde MS % carbo.xlsx, carb Page 1 of 1 EA# B Page 4 of 97 09/16/ :03

5 Report for: For the benefit of VaporFi, Inc. Project Code: Client Project: RM02 & HPHC Testing Project Start Date: 08/07/2014 Sample Type: eliquid Analysis Method: GC/MS/MS Enthalpy Code Client Code 1-ANP (ng/ml) 2-ANP (ng/ml) 4-ABP (ng/ml) an4 (ug/ml) RM < 1.81 ND < 1.80 ND < ND < 1.10 ND ND: Not Detected; analytes not detected above the minimum detection limit. Compound / MS Sample Spiked Native Recovery Sample ID (ng) (ng) (ng) % 1-ANP MS % 2-ANP MS % 4-ABP MS % ND: Not Detected; analytes not detected above the minimum detection limit. Analyte Code 1-ANP: 1-Aminonaphthalene 2-ANP: 2-Aminonaphthalene 4-ABP: 4-Aminobiphenyl B eliq ArAm.xlsx, AA Page 1 of 1 EA# B Page 5 of 97 09/16/ :39

6 Narrative Summary EA# B Page 6 of 97

7 Enthalpy Analytical Narrative Summary Company For the benefit of VaporFi, Inc. Eliquid samples Analyst WJG / ETA Job # Parameters HPLC/UV Analysis # Samples 1 Custody Analysis Summer Mims received the samples on 8/7/14 after being relinquished by for the benefit of VaporFi, Inc. The samples were received at ambient temperature in good condition. Prior to, during, and after analysis, the samples were kept under lock with access only to authorized personnel by Enthalpy Analytical, Inc. The samples were analyzed for acetaldehyde, acrolein, crotonaldehyde, and formaldehyde following the analytical procedures in Enthalpy SOP ENT301. The Agilent Model 1100, High Performance Liquid Chromatograph "Groucho" was equipped with an Ultraviolet (UV) Detector operating at 365 nm and an appropriate column. Calibration QC Notes The calibration curve is located in the Carbonyls Raw Data section of this report. Acetaldehyde, acrolein, formaldehyde, and crotonaldehyde were not detected in the blank at levels above the minimum detection limit (MDL). A matrix spike (MS) was prepared using an aliquot of the sample. The recovery values were within 30% of the expected values. Reporting Notes The reported concentrations (ug/ml) were calculated by multiplying the diluted results by the dilution factor. The data in the Raw Data section of the report are diluted and have not been adjusted for the dilution factor. The results presented in this report are representative of the sample as provided to the laboratory. EA# B Page 7 of 97

8 Enthalpy Analytical Narrative Summary Company For the benefit of VaporFi, Inc. Eliquid samples Analyst SSB Job # Parameters GC/MS/MS Analysis # Samples 1 Custody Summer Mims received the samples on 8/7/14 after being relinquished by for the benefit of VaporFi, Inc. The samples were received at ambient temperature in good condition. Prior to, during, and after analysis, the samples were kept under lock with access only to authorized personnel by Enthalpy Analytical, Inc. Analysis The liquid samples were analyzed for 1-aminonaphthalene (1-ANP), 2- aminonaphthalene (2-ANP), and 4-aminobiphenyl (1-ABP) following the general analytical procedures for GC/MS analyses and Enthalpy SOP ENT213. Aliquots of 0.5 ml of each sample were combined with 4.5mL of HCl and 0.1mL of internal standard. The Agilent Model 7890A Gas Chromatograph Bender was coupled to an Agilent Model 5975 Mass Selective Detector and was fitted with an appropriate column. Calibration QC Notes Refer to the Aromatic Amines Raw Data section of this report for chromatograms. The target analytes were not detected in the laboratory blank or the sample above the MDL. A matrix spike (MS) was prepared using an aliquot of the sample. The recovery values were within 15% of the expected values Reporting Notes The reported < concentrations were calculated by dividing the MDL ng by the sample aliquot volume (0.5 ml) used for the analysis. The chromatograms in the Raw Data section of the report present the results in units of ng. The results presented in this report are representative of the samples as provided to the laboratory. EA# B Page 8 of 97

9 General Reporting Notes The following are general reporting notes that are applicable to all Enthalpy Analytical, Inc. data reports, unless specifically noted otherwise. Any analysis which refers to the method as Type represents a planned deviation from the reference method. For instance a Hydrogen Sulfide assay from a Tedlar bag would be labeled as EPA Method 16-Type because Tedlar bags are not mentioned as one of the collection options in EPA Method 16. The acronym MDL represents the Minimum Detection Limit. Below this value the laboratory cannot determine the presence of the analyte of interest reliably. The acronym LOQ represents the Limit of Quantification. Below this value the laboratory cannot quantitate the analyte of interest within the criteria of the method. The acronym ND following a value indicates a non-detect or analytical result below the MDL. The letter J in the Qualifier or Flag column in the results indicates that the value is between the MDL and the LOQ. The laboratory can positively identify the analyte of interest as present, but the value should be considered an estimate. The letter E in the Qualifier or Flag column indicates an analytical result exceeding 100% of the highest calibration point. The associated value should be considered as an estimate. The acronym DF represents Dilution Factor. This number represents dilution of the sample during the preparation and/or analysis process. The analytical result taken from a laboratory instrument is multiplied by the DF to determine the final undiluted sample results. The addition of MS to the Sample ID represents a Matrix Spike. An aliquot of an actual sample is spiked with a known amount of analyte so that a percent recovery value can be determined. The MS analysis indicates what effect the sample matrix may have on the target analyte, i.e. whether or not anything in the sample matrix interferes with the analysis of the analyte(s). The addition of MSD to the Sample ID represents a Matrix Spike Duplicate. Prepared in the same manner as a MS, the use of duplicate matrix spikes allows further confirmation of laboratory quality by showing the consistency of results gained by performing the same steps multiple times. The addition of LD to the Sample ID represents a Laboratory Duplicate. The analyst prepares an additional aliquot of sample for testing and the results of the duplicate analysis are compared to the initial result. The result should have a difference value of within 10% of the initial result (if the results of the original analysis are greater than the LOQ). The addition of AD to the Sample ID represents an Alternate Dilution. The analyst prepares an additional aliquot at a different dilution factor (usually double the initial factor). This analysis helps confirm that no additional compound is present and coeluting or sharing absorbance with the analyte of interest, as they would have a different response/absorbance than the analyte of interest. EA# B Page 9 of 97

10 General Reporting Notes (continued) The Sample ID LCS represents a Laboratory Control Sample. Clean matrix, similar to the client sample matrix, prepared and analyzed by the laboratory using the same reagents, spiking standards and procedures used for the client samples. The LCS is used to assess the control of the laboratory s analytical system. Whenever spikes are prepared for our client projects, two spikes are retained as LCSs. The LCSs are labeled with the associated project number and kept in-house at the appropriate temperature conditions. When the project samples are received for analysis, the LCSs are analyzed to confirm that the analyte could be recovered from the media, separate from the samples which were used on the project and which may have been affected by source matrix, sample collection and/or sample transport. Significant Figures: Where the reported value is much greater than unity (1.00) in the units expressed, the number is rounded to a whole number of units, rather than to 3 significant figures. For example, a value of 10, ug catch is rounded to 10,456 ug. There are five significant digits displayed, but no confidence should be placed on more than two significant digits. Manual Integration: The data systems used for processing will flag manually integrated peaks with an M. There are several reasons a peak may be manually integrated. These reasons will be identified by the following two letter designations on sample chromatograms, if provided in the report. The peak was not integrated by the software NI, the peak was integrated incorrectly by the software II or the wrong peak was integrated by the software WP. These codes will accompany the analyst s manual integration stamp placed next to the compound name on the chromatogram. EA# B Page 10 of 97

11 Sample Custody Record EA# B Page 11 of 97

12 For the benefit of VaporFi, Inc. EA# B Page 12 of 97

13 EA# B Page 13 of 97 Raw Data

14 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO126\ D /4/2014 1:19:20 AM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/ :37:58 PM Groucho GROUCHO126 Erik Alvarez Enthalpy Analytical, Inc. Sample type: Sample Location: 51 Injection volume: Injection: 1 of 1 File_Version 8 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Formaldehyde BB ug/ml Acetaldehyde VB ug/ml Acrolein ug/ml Crotonaldehyde ug/ml 4 cmpds GoodCat [Rev. 2] Printed: 09/11/ :09:06 Page 1 of 1 EA# B Page 14 of 97

15 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO126\ D DNPH Blank 9/4/2014 2:21:39 AM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/ :10:52 AM Groucho GROUCHO126 Erik Alvarez Enthalpy Analytical, Inc. Sample type: Sample Location: 53 Injection volume: Injection: 1 of 1 File_Version 7 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Formaldehyde ug/ml Acetaldehyde ug/ml Acrolein ug/ml Crotonaldehyde ug/ml 4 cmpds GoodCat [Rev. 1] Printed: 09/05/ :29:29 Page 2 of 6 EA# B Page 15 of 97

16 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO126\ D HPLC-STDs014 #4 9/4/2014 6:30:31 AM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/ :11:13 AM Groucho GROUCHO126 Erik Alvarez Enthalpy Analytical, Inc. Sample type: Calibration Location: 4 Injection volume: Injection: 1 of 1 File_Version 7 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Formaldehyde BB ug/ml Acetaldehyde BB ug/ml Acrolein BB ug/ml Crotonaldehyde BB ug/ml 4 cmpds GoodCat [Rev. 1] Printed: 09/05/ :29:29 Page 3 of 6 EA# B Page 16 of 97

17 Chromatogram Report Data file: C:\Chem32\1\DATA\GROUCHO127\ D Sample name: HPLC-STDs014 #4 File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: 9/5/ :52:29 AM Acq. method: ELIQUID_BC_NEW.M Analysis method: GROUCHO126.M Last changed: 9/5/2014 3:20:18 PM Instrument: Sequence_Name GROUCHO127 Acq. operator: Wendy Gardow Enthalpy Analytical, Inc. Sample type: Calibration Location: 4 Injection volume: Injection: 1 of 1 File_Version 2 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Formaldehyde BB ug/ml Acetaldehyde BB ug/ml Acrolein VB ug/ml Crotonaldehyde BB ug/ml 4 cmpds GoodCat [Rev. 1] Printed: 09/05/ :29:29 Page 4 of 6 EA# B Page 17 of 97

18 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO127\ D MS 9/5/ :25:58 PM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/2014 3:20:18 PM Groucho GROUCHO127 Wendy Gardow Enthalpy Analytical, Inc. Sample type: Sample Location: 72 Injection volume: Injection: 1 of 1 File_Version 2 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Formaldehyde VV ug/ml Acetaldehyde BB ug/ml Acrolein VV ug/ml Crotonaldehyde VB ug/ml 4 cmpds GoodCat [Rev. 1] Printed: 09/05/ :29:29 Page 5 of 6 EA# B Page 18 of 97

19 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO127\ D HPLC-STDs014 #4 9/5/ :57:09 PM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/2014 3:20:18 PM Groucho GROUCHO127 Wendy Gardow Enthalpy Analytical, Inc. Sample type: Calibration Location: 4 Injection volume: Injection: 1 of 1 File_Version 2 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Formaldehyde BB ug/ml Acetaldehyde BB ug/ml Acrolein VB ug/ml Crotonaldehyde BB ug/ml 4 cmpds GoodCat [Rev. 1] Printed: 09/05/ :29:29 Page 6 of 6 EA# B Page 19 of 97

20 Sequence Summary Report Sequence_AcquiredBy Sequence_AcquiredDate Sequence_Name Sequence_LastModifiedBy Erik Alvarez 9/3/2014 3:56:35 PM GROUCHO126 Wendy Gardow Sequence_Ver 6 Name Acetaldehyde Sample_ID Sample_Type Vial RT Area Dil Tag Amount Unit % of Amt Tag HPLC-STDs014 #1 Calibration ug/ml HPLC-STDs014 #2 Calibration ug/ml HPLC-STDs014 #3 Calibration ug/ml HPLC-STDs014 #4 Calibration ug/ml HPLC-STDs014 #5 Calibration ug/ml HPLC-STDs014 #6 Calibration ug/ml HPLC-STDs014 #7 Calibration ug/ml HPLC-STDs015 #1 Calibration ug/ml NaN HPLC-STDs015 #2 Calibration ug/ml NaN HPLC-STDs015 #3 Calibration ug/ml NaN HPLC-STDs015 #4 Calibration ug/ml NaN HPLC-STDs015 #5 Calibration ug/ml NaN HPLC-STDs015 #6 Calibration ug/ml NaN HPLC-STDs015 #7 Calibration ug/ml NaN Name Acetoin Sample_ID Sample_Type Vial RT Area Dil Tag Amt Amount Unit % of Tag HPLC-STDs014 #1 Calibration ug/ml NaN HPLC-STDs014 #2 Calibration ug/ml NaN HPLC-STDs014 #3 Calibration ug/ml NaN HPLC-STDs014 #4 Calibration ug/ml NaN HPLC-STDs014 #5 Calibration ug/ml NaN HPLC-STDs014 #6 Calibration ug/ml NaN HPLC-STDs014 #7 Calibration ug/ml NaN HPLC-STDs015 #1 Calibration ug/ml HPLC-STDs015 #2 Calibration ug/ml HPLC-STDs015 #3 Calibration ug/ml HPLC-STDs015 #4 Calibration ug/ml HPLC-STDs015 #5 Calibration ug/ml HPLC-STDs015 #6 Calibration ug/ml HPLC-STDs015 #7 Calibration ug/ml Name Acetone Summary with % Tag [Rev. 3] Printed: 09/05/ :14:06 Page 1 of 1 EA# B Page 20 of 97

21 Sequence Summary Report Sample_ID Sample_Type Vial RT Area Dil Tag Amount Unit % of Amt Tag HPLC-STDs014 #1 Calibration ug/ml HPLC-STDs014 #2 Calibration ug/ml HPLC-STDs014 #3 Calibration ug/ml HPLC-STDs014 #4 Calibration ug/ml HPLC-STDs014 #5 Calibration ug/ml HPLC-STDs014 #6 Calibration ug/ml HPLC-STDs014 #7 Calibration ug/ml HPLC-STDs015 #1 Calibration ug/ml NaN HPLC-STDs015 #2 Calibration ug/ml NaN HPLC-STDs015 #3 Calibration ug/ml NaN HPLC-STDs015 #4 Calibration ug/ml NaN HPLC-STDs015 #5 Calibration ug/ml NaN HPLC-STDs015 #6 Calibration ug/ml NaN HPLC-STDs015 #7 Calibration ug/ml NaN Name Acrolein Sample_ID Sample_Type Vial RT Area Dil Tag Amt Amount Unit % of Tag HPLC-STDs014 #1 Calibration ug/ml HPLC-STDs014 #2 Calibration ug/ml HPLC-STDs014 #3 Calibration ug/ml HPLC-STDs014 #4 Calibration ug/ml HPLC-STDs014 #5 Calibration ug/ml HPLC-STDs014 #6 Calibration ug/ml HPLC-STDs014 #7 Calibration ug/ml HPLC-STDs015 #1 Calibration ug/ml NaN HPLC-STDs015 #2 Calibration ug/ml NaN HPLC-STDs015 #3 Calibration ug/ml NaN HPLC-STDs015 #4 Calibration ug/ml NaN HPLC-STDs015 #5 Calibration ug/ml NaN HPLC-STDs015 #6 Calibration ug/ml NaN HPLC-STDs015 #7 Calibration ug/ml NaN Name Crotonaldehyde Sample_ID Sample_Type Vial RT Area Dil Tag Amount Unit % of Amt Tag HPLC-STDs014 #1 Calibration ug/ml HPLC-STDs014 #2 Calibration ug/ml HPLC-STDs014 #3 Calibration ug/ml HPLC-STDs014 #4 Calibration ug/ml HPLC-STDs014 #5 Calibration ug/ml HPLC-STDs014 #6 Calibration ug/ml HPLC-STDs014 #7 Calibration ug/ml HPLC-STDs015 #1 Calibration ug/ml NaN HPLC-STDs015 #2 Calibration ug/ml NaN HPLC-STDs015 #3 Calibration ug/ml NaN HPLC-STDs015 #4 Calibration ug/ml NaN HPLC-STDs015 #5 Calibration ug/ml NaN HPLC-STDs015 #6 Calibration ug/ml NaN HPLC-STDs015 #7 Calibration ug/ml NaN Name Diacetyl Summary with % Tag [Rev. 3] Printed: 09/05/ :14:06 Page 1 of 1 EA# B Page 21 of 97

22 Sequence Summary Report Sample_ID Sample_Type Vial RT Area Dil Tag Amt Amount Unit % of Tag HPLC-STDs014 #1 Calibration ug/ml NaN HPLC-STDs014 #2 Calibration ug/ml NaN HPLC-STDs014 #3 Calibration ug/ml NaN HPLC-STDs014 #4 Calibration ug/ml NaN HPLC-STDs014 #5 Calibration ug/ml NaN HPLC-STDs014 #6 Calibration ug/ml NaN HPLC-STDs014 #7 Calibration ug/ml NaN HPLC-STDs015 #1 Calibration ug/ml HPLC-STDs015 #2 Calibration ug/ml HPLC-STDs015 #3 Calibration ug/ml HPLC-STDs015 #4 Calibration ug/ml HPLC-STDs015 #5 Calibration ug/ml HPLC-STDs015 #6 Calibration ug/ml HPLC-STDs015 #7 Calibration ug/ml Name Formaldehyde Sample_ID Sample_Type Vial RT Area Dil Tag Amount Unit % of Amt Tag HPLC-STDs014 #1 Calibration ug/ml HPLC-STDs014 #2 Calibration ug/ml HPLC-STDs014 #3 Calibration ug/ml HPLC-STDs014 #4 Calibration ug/ml HPLC-STDs014 #5 Calibration ug/ml HPLC-STDs014 #6 Calibration ug/ml HPLC-STDs014 #7 Calibration ug/ml HPLC-STDs015 #1 Calibration ug/ml NaN HPLC-STDs015 #2 Calibration ug/ml NaN HPLC-STDs015 #3 Calibration ug/ml NaN HPLC-STDs015 #4 Calibration ug/ml NaN HPLC-STDs015 #5 Calibration ug/ml NaN HPLC-STDs015 #6 Calibration ug/ml NaN HPLC-STDs015 #7 Calibration ug/ml NaN Name Pentanedione Sample_ID Sample_Type Vial RT Area Dil Tag Amt Amount Unit % of Tag HPLC-STDs014 #1 Calibration ug/ml NaN HPLC-STDs014 #2 Calibration ug/ml NaN HPLC-STDs014 #3 Calibration ug/ml NaN HPLC-STDs014 #4 Calibration ug/ml NaN HPLC-STDs014 #5 Calibration ug/ml NaN HPLC-STDs014 #6 Calibration ug/ml NaN HPLC-STDs014 #7 Calibration ug/ml NaN HPLC-STDs015 #1 Calibration ug/ml HPLC-STDs015 #2 Calibration ug/ml HPLC-STDs015 #3 Calibration ug/ml HPLC-STDs015 #4 Calibration ug/ml HPLC-STDs015 #5 Calibration ug/ml HPLC-STDs015 #6 Calibration ug/ml HPLC-STDs015 #7 Calibration ug/ml Summary with % Tag [Rev. 3] Printed: 09/05/ :14:06 Page 1 of 1 EA# B Page 22 of 97

23 Sequence Summary Report Sequence_AcquiredBy Sequence_AcquiredDate Sequence_Name Sequence_LastModifiedBy Erik Alvarez 9/3/2014 3:56:35 PM GROUCHO126 Wendy Gardow Sequence_Ver 6 Name Acetaldehyde Sample_ID Sample_Type Vial RT Area Dil Amount Unit HPLC-STDs014 #SS Control ug/ml HPLC-STDs014 #RB Control ug/ml HPLC-STDs015 #SS Control ug/ml HPLC-STDs015 #RB Control ug/ml Name Acetoin Sample_ID Sample_Type Vial RT Area Dil Amount Unit HPLC-STDs014 #SS Control ug/ml HPLC-STDs014 #RB Control ug/ml HPLC-STDs015 #SS Control ug/ml HPLC-STDs015 #RB Control ug/ml Name Acetone Sample_ID Sample_Type Vial RT Area Dil Amount Unit HPLC-STDs014 #SS Control ug/ml HPLC-STDs014 #RB Control ug/ml HPLC-STDs015 #SS Control ug/ml HPLC-STDs015 #RB Control ug/ml Name Acrolein Sample_ID Sample_Type Vial RT Area Dil Amount Unit HPLC-STDs014 #SS Control ug/ml HPLC-STDs014 #RB Control ug/ml HPLC-STDs015 #SS Control ug/ml HPLC-STDs015 #RB Control ug/ml Name Crotonaldehyde Sample_ID Sample_Type Vial RT Area Dil Amount Unit HPLC-STDs014 #SS Control ug/ml HPLC-STDs014 #RB Control ug/ml HPLC-STDs015 #SS Control ug/ml HPLC-STDs015 #RB Control ug/ml Name Diacetyl Sample_ID Sample_Type Vial RT Area Dil Amount Unit HPLC-STDs014 #SS Control ug/ml HPLC-STDs014 #RB Control ug/ml HPLC-STDs015 #SS Control ug/ml HPLC-STDs015 #RB Control ug/ml Name Formaldehyde Sample_ID Sample_Type Vial RT Area Dil Amount Unit HPLC-STDs014 #SS Control ug/ml HPLC-STDs014 #RB Control ug/ml HPLC-STDs015 #SS Control ug/ml HPLC-STDs015 #RB Control ug/ml Name Pentanedione Summary with % Tag [Rev. 3] Printed: 09/05/ :14:06 Page 1 of 1 EA# B Page 23 of 97

24 Sequence Summary Report Sample_ID HPLC-STDs014 #SS HPLC-STDs014 #RB Sample_Type Control Control Vial 8 9 RT Area Dil 1 1 Amount Unit ug/ml ug/ml HPLC-STDs015 #SS HPLC-STDs015 #RB Control Control ug/ml ug/ml Compound Acetaldehyde : Signal: Exp. RT: Corr Coeff : Residual: RF RSD%: Formula: y = ax + b a: b: c: d: VWD1A Compound Acetoin : Signal: Exp. RT: Corr Coeff : Residual: RF RSD%: Formula: y = ax + b a: b: c: d: VWD1A Summary with % Tag [Rev. 3] Printed: 09/05/ :14:06 Page 1 of 1 EA# B Page 24 of 97

25 Sequence Summary Report Compound Acetone : Signal: Exp. RT: Corr Coeff : Residual: RF RSD%: Formula: y = ax + b a: b: c: d: VWD1A Compound Acrolein : Signal: Exp. RT: Corr Coeff : Residual: RF RSD%: Formula: y = ax + b a: b: c: d: VWD1A Summary with % Tag [Rev. 3] Printed: 09/05/ :14:06 Page 1 of 1 EA# B Page 25 of 97

26 Sequence Summary Report Compound Crotonaldehyde : Signal: VWD1A Exp. RT: Corr Coeff : Residual: RF RSD%: Formula: y = ax + b a: b: c: d: Compound Diacetyl : Signal: Exp. RT: Corr Coeff : Residual: RF RSD%: Formula: y = ax + b a: b: c: d: VWD1A Summary with % Tag [Rev. 3] Printed: 09/05/ :14:06 Page 1 of 1 EA# B Page 26 of 97

27 Sequence Summary Report Compound Formaldehyde : Signal: Exp. RT: Corr Coeff : Residual: RF RSD%: Formula: y = ax + b a: b: c: d: VWD1A Compound Pentanedione : Signal: Exp. RT: Corr Coeff : Residual: RF RSD%: Formula: y = ax + b a: b: c: d: VWD1A Summary with % Tag [Rev. 3] Printed: 09/05/ :14:06 Page 1 of 1 EA# B Page 27 of 97

28 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO126\ D HPLC-STDs014 #1 9/3/2014 3:58:25 PM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/ :13:15 AM Groucho GROUCHO126 Erik Alvarez Enthalpy Analytical, Inc. Sample type: Calibration Location: 1 Injection volume: Injection: 1 of 1 File_Version 7 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Acetoin ug/ml Formaldehyde BB ug/ml Acetaldehyde MM ug/ml Diacetyl ug/ml Acetone BB ug/ml Acrolein BB ug/ml Pentanedione ug/ml Crotonaldehyde BB ug/ml all carbs [Rev. 3] Printed: 09/05/ :18:40 Page 1 of 18 EA# B Page 28 of 97

29 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO126\ D HPLC-STDs014 #2 9/3/2014 4:29:31 PM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/ :10:52 AM Groucho GROUCHO126 Erik Alvarez Enthalpy Analytical, Inc. Sample type: Calibration Location: 2 Injection volume: Injection: 1 of 1 File_Version 7 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Acetoin ug/ml Formaldehyde BB ug/ml Acetaldehyde MM ug/ml Diacetyl ug/ml Acetone BB ug/ml Acrolein BB ug/ml Pentanedione ug/ml Crotonaldehyde BB ug/ml all carbs [Rev. 3] Printed: 09/05/ :18:40 Page 2 of 18 EA# B Page 29 of 97

30 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO126\ D HPLC-STDs014 #3 9/3/2014 5:00:43 PM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/ :10:52 AM Groucho GROUCHO126 Erik Alvarez Enthalpy Analytical, Inc. Sample type: Calibration Location: 3 Injection volume: Injection: 1 of 1 File_Version 7 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Acetoin ug/ml Formaldehyde BB ug/ml Acetaldehyde BB ug/ml Diacetyl ug/ml Acetone BB ug/ml Acrolein BB ug/ml Pentanedione ug/ml Crotonaldehyde BB ug/ml all carbs [Rev. 3] Printed: 09/05/ :18:40 Page 3 of 18 EA# B Page 30 of 97

31 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO126\ D HPLC-STDs014 #4 9/3/2014 5:31:49 PM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/ :10:52 AM Groucho GROUCHO126 Erik Alvarez Enthalpy Analytical, Inc. Sample type: Calibration Location: 4 Injection volume: Injection: 1 of 1 File_Version 7 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Acetoin ug/ml Formaldehyde BB ug/ml Acetaldehyde BB ug/ml Diacetyl ug/ml Acetone BB ug/ml Acrolein BB ug/ml Pentanedione ug/ml Crotonaldehyde BB ug/ml all carbs [Rev. 3] Printed: 09/05/ :18:40 Page 4 of 18 EA# B Page 31 of 97

32 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO126\ D HPLC-STDs014 #5 9/3/2014 6:03:16 PM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/ :10:52 AM Groucho GROUCHO126 Erik Alvarez Enthalpy Analytical, Inc. Sample type: Calibration Location: 5 Injection volume: Injection: 1 of 1 File_Version 7 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Acetoin ug/ml Formaldehyde BB ug/ml Acetaldehyde BB ug/ml Diacetyl ug/ml Acetone BV ug/ml Acrolein VB ug/ml Pentanedione ug/ml Crotonaldehyde BB ug/ml all carbs [Rev. 3] Printed: 09/05/ :18:40 Page 5 of 18 EA# B Page 32 of 97

33 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO126\ D HPLC-STDs014 #6 9/3/2014 6:34:26 PM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/ :10:52 AM Groucho GROUCHO126 Erik Alvarez Enthalpy Analytical, Inc. Sample type: Calibration Location: 6 Injection volume: Injection: 1 of 1 File_Version 7 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Acetoin ug/ml Formaldehyde BB ug/ml Acetaldehyde BB ug/ml Diacetyl ug/ml Acetone BV ug/ml Acrolein VB ug/ml Pentanedione ug/ml Crotonaldehyde BB ug/ml all carbs [Rev. 3] Printed: 09/05/ :18:40 Page 6 of 18 EA# B Page 33 of 97

34 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO126\ D HPLC-STDs014 #7 9/3/2014 7:05:33 PM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/ :10:52 AM Groucho GROUCHO126 Erik Alvarez Enthalpy Analytical, Inc. Sample type: Calibration Location: 7 Injection volume: Injection: 1 of 1 File_Version 7 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Acetoin ug/ml Formaldehyde BB ug/ml Acetaldehyde BB ug/ml Diacetyl ug/ml Acetone BV ug/ml Acrolein VB ug/ml Pentanedione ug/ml Crotonaldehyde BB ug/ml all carbs [Rev. 3] Printed: 09/05/ :18:40 Page 7 of 18 EA# B Page 34 of 97

35 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO126\ D HPLC-STDs014 #SS 9/3/2014 7:36:42 PM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/ :10:52 AM Groucho GROUCHO126 Erik Alvarez Enthalpy Analytical, Inc. Sample type: Control Location: 8 Injection volume: Injection: 1 of 1 File_Version 7 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Acetoin ug/ml Formaldehyde BB ug/ml Acetaldehyde BB ug/ml Diacetyl ug/ml Acetone BB ug/ml Acrolein BB ug/ml Pentanedione ug/ml Crotonaldehyde BB ug/ml all carbs [Rev. 3] Printed: 09/05/ :18:40 Page 8 of 18 EA# B Page 35 of 97

36 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO126\ D HPLC-STDs014 #RB 9/3/2014 8:07:53 PM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/ :10:52 AM Groucho GROUCHO126 Erik Alvarez Enthalpy Analytical, Inc. Sample type: Control Location: 9 Injection volume: Injection: 1 of 1 File_Version 7 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Acetoin ug/ml Formaldehyde ug/ml Acetaldehyde ug/ml Diacetyl ug/ml Acetone ug/ml Acrolein ug/ml Pentanedione ug/ml Crotonaldehyde ug/ml all carbs [Rev. 3] Printed: 09/05/ :18:40 Page 9 of 18 EA# B Page 36 of 97

37 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO126\ D HPLC-STDs015 #1 9/3/2014 8:39:04 PM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/ :10:52 AM Groucho GROUCHO126 Erik Alvarez Enthalpy Analytical, Inc. Sample type: Calibration Location: 91 Injection volume: Injection: 1 of 1 File_Version 7 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Acetoin BB ug/ml Formaldehyde ug/ml Acetaldehyde ug/ml Diacetyl BB ug/ml Acetone ug/ml Acrolein ug/ml Pentanedione BB ug/ml Crotonaldehyde ug/ml all carbs [Rev. 3] Printed: 09/05/ :18:40 Page 10 of 18 EA# B Page 37 of 97

38 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO126\ D HPLC-STDs015 #2 9/3/2014 9:10:12 PM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/ :10:52 AM Groucho GROUCHO126 Erik Alvarez Enthalpy Analytical, Inc. Sample type: Calibration Location: 92 Injection volume: Injection: 1 of 1 File_Version 7 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Acetoin BB ug/ml Formaldehyde ug/ml Acetaldehyde ug/ml Diacetyl BB ug/ml Acetone ug/ml Acrolein ug/ml Pentanedione BB ug/ml Crotonaldehyde ug/ml all carbs [Rev. 3] Printed: 09/05/ :18:40 Page 11 of 18 EA# B Page 38 of 97

39 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO126\ D HPLC-STDs015 #3 9/3/2014 9:41:22 PM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/ :10:52 AM Groucho GROUCHO126 Erik Alvarez Enthalpy Analytical, Inc. Sample type: Calibration Location: 93 Injection volume: Injection: 1 of 1 File_Version 7 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Acetoin BB ug/ml Formaldehyde ug/ml Acetaldehyde ug/ml Diacetyl BB ug/ml Acetone ug/ml Acrolein ug/ml Pentanedione BV ug/ml Crotonaldehyde ug/ml all carbs [Rev. 3] Printed: 09/05/ :18:40 Page 12 of 18 EA# B Page 39 of 97

40 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO126\ D HPLC-STDs015 #4 9/3/ :12:30 PM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/ :10:52 AM Groucho GROUCHO126 Erik Alvarez Enthalpy Analytical, Inc. Sample type: Calibration Location: 94 Injection volume: Injection: 1 of 1 File_Version 7 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Acetoin BB ug/ml Formaldehyde ug/ml Acetaldehyde ug/ml Diacetyl BB ug/ml Acetone ug/ml Acrolein ug/ml Pentanedione BV ug/ml Crotonaldehyde ug/ml all carbs [Rev. 3] Printed: 09/05/ :18:40 Page 13 of 18 EA# B Page 40 of 97

41 Chromatogram Report Data file: C:\Chem32\1\DATA\GROUCHO126\ D Sample name: HPLC-STDs015 #5 File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: 9/3/ :43:40 PM Acq. method: ELIQUID_BC_NEW.M Analysis method: GROUCHO126.M Last changed: 9/5/ :10:52 AM Instrument: Sequence_Name GROUCHO126 Acq. operator: Erik Alvarez Enthalpy Analytical, Inc. Sample type: Calibration Location: 95 Injection volume: Injection: 1 of 1 File_Version 7 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Acetoin BV ug/ml Formaldehyde ug/ml Acetaldehyde ug/ml Diacetyl BB ug/ml Acetone ug/ml Acrolein ug/ml Pentanedione BV ug/ml Crotonaldehyde ug/ml all carbs [Rev. 3] Printed: 09/05/ :18:40 Page 14 of 18 EA# B Page 41 of 97

42 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO126\ D HPLC-STDs015 #6 9/3/ :14:45 PM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/ :10:52 AM Groucho GROUCHO126 Erik Alvarez Enthalpy Analytical, Inc. Sample type: Calibration Location: 96 Injection volume: Injection: 1 of 1 File_Version 7 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Acetoin BV ug/ml Formaldehyde ug/ml Acetaldehyde ug/ml Diacetyl BB ug/ml Acetone ug/ml Acrolein ug/ml Pentanedione VV ug/ml Crotonaldehyde ug/ml all carbs [Rev. 3] Printed: 09/05/ :18:40 Page 15 of 18 EA# B Page 42 of 97

43 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO126\ D HPLC-STDs015 #7 9/3/ :45:55 PM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/ :10:52 AM Groucho GROUCHO126 Erik Alvarez Enthalpy Analytical, Inc. Sample type: Calibration Location: 97 Injection volume: Injection: 1 of 1 File_Version 7 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Acetoin BV ug/ml Formaldehyde ug/ml Acetaldehyde ug/ml Diacetyl BB ug/ml Acetone ug/ml Acrolein ug/ml Pentanedione VV ug/ml Crotonaldehyde ug/ml all carbs [Rev. 3] Printed: 09/05/ :18:40 Page 16 of 18 EA# B Page 43 of 97

44 Chromatogram Report Data file: Sample name: File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\Chem32\1\DATA\GROUCHO126\ D HPLC-STDs015 #SS 9/4/ :17:06 AM ELIQUID_BC_NEW.M GROUCHO126.M 9/5/ :10:52 AM Groucho GROUCHO126 Erik Alvarez Enthalpy Analytical, Inc. Sample type: Control Location: 98 Injection volume: Injection: 1 of 1 File_Version 7 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Acetoin BV ug/ml Formaldehyde ug/ml Acetaldehyde VB ug/ml Diacetyl BB ug/ml Acetone BB ug/ml Acrolein ug/ml Pentanedione BV ug/ml Crotonaldehyde ug/ml all carbs [Rev. 3] Printed: 09/05/ :18:40 Page 17 of 18 EA# B Page 44 of 97

45 Chromatogram Report Data file: C:\Chem32\1\DATA\GROUCHO126\ D Sample name: HPLC-STDs015 #RB File_Location \TSC Data\2014\Groucho\Quarter 3 Injection date: 9/4/ :48:09 AM Acq. method: ELIQUID_BC_NEW.M Analysis method: GROUCHO126.M Last changed: 9/5/ :10:52 AM Instrument: Sequence_Name GROUCHO126 Acq. operator: Erik Alvarez Enthalpy Analytical, Inc. Sample type: Control Location: 99 Injection volume: Injection: 1 of 1 File_Version 7 Name Peak_Type RT [min] Area Dil ug/ml Sample_Amount Units Acetoin ug/ml Formaldehyde ug/ml Acetaldehyde ug/ml Diacetyl ug/ml Acetone ug/ml Acrolein ug/ml Pentanedione ug/ml Crotonaldehyde ug/ml all carbs [Rev. 3] Printed: 09/05/ :18:40 Page 18 of 18 EA# B Page 45 of 97

46 EA# B Page 46 of 97 Raw Data

47 Quantitative Analysis Summary Report Batch Data Path D:\Data\MS2014Q3\Bender\data\sep14\Bender p0046\quantresults\bender p ArAm eliq.batch.bin Analysis Time 9/16/ :28 AM Analyst Name EAINC\SBrown Report Time 9/16/ :29 AM Reporter Name EAINC\SBrown Last Calib Update 9/16/ :28 AM Batch State Processed T11:28: : T11:29: : T11:28: :00 Quantitation Results Target Compound 1-ANP SampleName Sample Type LevelName Data File AcqDateTime Compound Exp Conc (ng) Dilution Final Conc (ng) Accuracy 2nd An. Review toluene blk DoubleBlank B D T11:3 1-ANP LAH ArAm ISTD blk Blank B D T11:4 1-ANP 1 0 LAH ArAm Std 1 Calibration 1 B D T11:5 1-ANP LAH ArAm Std 3 Calibration 3 B D T12:1 1-ANP LAH ArAm Std 4 Calibration 4 B D T12:2 1-ANP LAH ArAm Std 5 Calibration 5 B D T12:3 1-ANP LAH ArAm ISTD blk Blank B D T12:4 1-ANP 1 0 LAH ArAm SS Std QC SS B D T12:5 1-ANP LAH Concal (ArAm Std 4) QC 4 B D T13:1 1-ANP LAH Concal (ArAm Std 4) QC 4 B D T10:1 1-ANP LAH Sample B D T14:0 1-ANP 1 0 LAH MS QC LCS B D T14:2 1-ANP LAH LCS-01 QC LCS B D T14:3 1-ANP LAH ArAm Blk-01 Sample B D T14:4 1-ANP 1 0 LAH Concal (ArAm Std 4) QC 4 B D T14:5 1-ANP LAH Target Compound 2-ANP SampleName Sample Type LevelName Data File AcqDateTime Compound Exp Conc (ng) Dilution Final Conc (ng) Accuracy 2nd An. Review toluene blk DoubleBlank B D T11:3 2-ANP LAH ArAm ISTD blk Blank B D T11:4 2-ANP 1 0 LAH ArAm Std 1 Calibration 1 B D T11:5 2-ANP LAH ArAm Std 3 Calibration 3 B D T12:1 2-ANP LAH ArAm Std 4 Calibration 4 B D T12:2 2-ANP LAH ArAm Std 5 Calibration 5 B D T12:3 2-ANP LAH ArAm ISTD blk Blank B D T12:4 2-ANP 1 0 LAH ArAm SS Std QC SS B D T12:5 2-ANP LAH Concal (ArAm Std 4) QC 4 B D T13:1 2-ANP LAH Concal (ArAm Std 4) QC 4 B D T10:1 2-ANP LAH Sample B D T14:0 2-ANP 1 0 LAH MS QC LCS B D T14:2 2-ANP LAH LCS-01 QC LCS B D T14:3 2-ANP LAH ArAm Blk-01 Sample B D T14:4 2-ANP 1 0 LAH Concal (ArAm Std 4) QC 4 B D T14:5 2-ANP LAH Target Compound 4-ABP Bemder p ArAm eliq reviewed.xlsx Page 1 of 50 Printed at: 11:38 AM on: 9/16/2014 EA# B Page 47 of 97

48 Quantitative Analysis Summary Report SampleName Sample Type LevelName Data File AcqDateTime Compound Exp Conc (ng) Dilution Final Conc (ng) Accuracy 2nd An. Review toluene blk DoubleBlank B D T11:3 4-ABP LAH ArAm ISTD blk Blank B D T11:4 4-ABP 1 0 LAH ArAm Std 1 Calibration 1 B D T11:5 4-ABP LAH ArAm Std 3 Calibration 3 B D T12:1 4-ABP LAH ArAm Std 4 Calibration 4 B D T12:2 4-ABP LAH ArAm Std 5 Calibration 5 B D T12:3 4-ABP LAH ArAm ISTD blk Blank B D T12:4 4-ABP 1 0 LAH ArAm SS Std QC SS B D T12:5 4-ABP LAH Concal (ArAm Std 4) QC 4 B D T13:1 4-ABP LAH Concal (ArAm Std 4) QC 4 B D T10:1 4-ABP LAH Sample B D T14:0 4-ABP 1 0 LAH MS QC LCS B D T14:2 4-ABP LAH LCS-01 QC LCS B D T14:3 4-ABP LAH ArAm Blk-01 Sample B D T14:4 4-ABP 1 0 LAH Concal (ArAm Std 4) QC 4 B D T14:5 4-ABP LAH Bemder p ArAm eliq reviewed.xlsx Page 2 of 50 Printed at: 11:38 AM on: 9/16/2014 EA# B Page 48 of 97

49 Quantitative Analysis Calibration Report Batch Data Path D:\Data\MS2014Q3\Bender\data\sep14\Bender p0046\quantresults\bender p ArAm eli Analysis Time 9/16/ :28 AM Analyst Name EAINC\SBrown Report Time 9/16/ :29 AM Reporter Name EAINC\SBrown Last Calib Update 9/16/ :28 AM Batch State Processed T11:28: : T11:29: : T11:28: :00 Calibration Info ISTD Compound 1-ANP-d7 Calibration STD Cal Type Level Enabled Response Exp Conc RF D:\Data\MS2014Q3\Bender\dataCalibration D:\Data\MS2014Q3\Bender\dataCalibration D:\Data\MS2014Q3\Bender\dataCalibration D:\Data\MS2014Q3\Bender\dataQC D:\Data\MS2014Q3\Bender\dataQC D:\Data\MS2014Q3\Bender\dataQC D:\Data\MS2014Q3\Bender\dataCalibration D:\Data\MS2014Q3\Bender\dataQC LCS D:\Data\MS2014Q3\Bender\dataQC LCS D:\Data\MS2014Q3\Bender\dataQC SS Target Compound 1-ANP Calibration STD Cal Type Level Enabled Response Exp Conc RF D:\Data\MS2014Q3\Bender\dataCalibration D:\Data\MS2014Q3\Bender\dataCalibration D:\Data\MS2014Q3\Bender\dataCalibration D:\Data\MS2014Q3\Bender\dataQC D:\Data\MS2014Q3\Bender\dataQC D:\Data\MS2014Q3\Bender\dataQC D:\Data\MS2014Q3\Bender\dataCalibration D:\Data\MS2014Q3\Bender\dataQC LCS D:\Data\MS2014Q3\Bender\dataQC LCS D:\Data\MS2014Q3\Bender\dataQC SS ISTD Compound 2-ANP-d7 Calibration STD Cal Type Level Enabled Response Exp Conc RF Bemder p ArAm eliq reviewed.xlsx Page 3 of 50 Printed at: 11:38 AM on: 9/16/2014 EA# B Page 49 of 97