e-liquid Samples Received 05/16/2014 Analysis Report ( ) GC/FID Analysis Nicotine Diethy lene glycol (DEG)

Size: px

Start display at page:

Download "e-liquid Samples Received 05/16/2014 Analysis Report ( ) GC/FID Analysis Nicotine Diethy lene glycol (DEG)"

Edgar Bennett
5 years ago
Views:

1 e-liquid Samples Received 05/16/2014 Analysis Report ( ) GC/FID Analysis Nicotine Diethy lene glycol (DEG) HBLCIUV Analysis Acetaldehyde Aceto in Diacetyl Formaldehyde Pentanedione Karl Fischer Analysis % Water Enthalpy Analytical, Inc Capitola Drive Durham, NC

I certify t hat 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

2 I certify t hat 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 t hat all deviations and analytical problems are summarized in the appropriate narrative(s) This analytical report was prepared in Portable Document Format (.PDF) and contains 33 pages. EA# Page 2 of 33

3 EA# Page 3 of 33

0514-132-01-02 Nicotine (mg/ml) 22.6 22.4 22.5 O.i7 12.4 12.

4 ACCREDI T ED Testing Cert. # Report for: Client Project: ECTA of Canada Sample Type: eliquid Project Code: Project Start Date: Analysis Method: /16/2014 ENT184 Enthalpy Code Nicotine (mg/ml) O.i < 0.1 ND < 0.1 ND v0.1 nic.xlsx, 132 Page 1 of 1 EA# Page 4 of 33

Company: Client Project: - Sample Type: eliquid Project Code: 0514-132 Project Start

Diethylene glycol (ug/ml) 0514-132-01-01 0514-132-01-02 < 2.23 ND < 2.

5 Company: Client Project: - Sample Type: eliquid Project Code: Project Start Date: 05/16/2014 Analysis Methods: ENT184 Enthalpy Code Client Code Lot# I Notes Diethylene glycol (ug/ml) < 2.23 ND < 2.23 ND NA NA < 2.23 ND < 2.23 ND Average % Diff EA# Page 5 of 33

Report for: Client Project: - Sample Type: eliquid Project Code: Project Start Date: Analysis Method: 0514-132 05/16/2014 ENT303 Enthalpy Code Client Code Acetaldehyde (ug/ml) Acetoin Diacetyl

6 Report for: Client Project: - Sample Type: eliquid Project Code: Project Start Date: Analysis Method: /16/2014 ENT303 Enthalpy Code Client Code Acetaldehyde (ug/ml) Acetoin Diacetyl Formaldehyde (ug/ml ) (ug/ml) (ug/ml) Pentanedione (ug/ml) J 19.9 < ND < ND J J 1.15 J < ND 1.28 J < ND 7.60 < ND ND: Non Detect or analytical result below the MDL and is less than (<)the reported value. J: Results flagged "J" are below the Lower Curve Limit, above the MDL, and are considered estimates gen v0.3 carb.xlsx, 132 Page 1 of 1 EA# Page 6 of 33

Project Code: 0514-132 Project Start Date: 05/16/2014 Analysis Methods: ENT058 & 072

7 Project Code: Project Start Date: 05/16/2014 Analysis Methods: ENT058 & 072 Enthalpy Code % Water ph-kft.xlsx, Water-pH all Page 1 of 1 EA# Page 7 of 33

8 EA# Page 8 of 33

Joli# 0514-132 EN 184, ENT30~Karl Fischer Titration, ph Custody Chester Burnett received samples on 5/16/14 after being relinhuished by Vapemate.

Hrior to, during, and after analysis, the samples were kept under lock with ccess only to authorized personnel by Entllal_p,M Arialytical, Inc. Th 1i uid samples were prepared anu ap.

$The Hewlett Packard Model 5890 Series Ir Gas <rhromafograph \\"Rickyn SIN 3336A52 180) was equipped with a FID and an appropriate column. The samples were prerared an1 analyzed for diethylene &!$

9 Joli# EN 184, ENT30~Karl Fischer Titration, ph Custody Chester Burnett received samples on 5/16/14 after being relinhuished by Vapemate. The samples Were received at ambient temperature in good condition. Hrior to, during, and after analysis, the samples were kept under lock with ccess only to authorized personnel by Entllal_p,M Arialytical, Inc. Th 1i uid samples were prepared anu ap.alyzed for nicotine follo h ng the anal)1ical procedures in Enthalpy SOP ENT 184. The Hewlett Packard Model 5890 Series Ir Gas <rhromafograph \\"Rickyn SIN 3336A52 180) was equipped with a FID and an appropriate column. The samples were prerared an1 analyzed for diethylene &!ycol (DEG) following the analytical procedures in Enthalpy SOP ENT 184 The Hewlett PaGkard Model 5890, Series II Gas Chromatograph "Teller" was equipped 'with a Flame Ionization Detector and an app opriate column.. The iquid samples were analyzed for acetaldehyde, acetoin, diacetyl, formal~eliyde, and pentanedione following t9e procedures in Enthalpy SOP-ENT303..,. The samples w.ere. analyzed using the Agilent Mo~el 1100: High Performance Liquia Chromatograph "Selma" equipped with an Ultraviolet (UV) Detector operating at 365 nm and an appropriate izolumn. Samples were measured for ph' using an Orion 230A ph m_eter. Each sample was diluted to a 1% aqueous solution with DI water. Samples were analyzed for water content using the analytical procedures in Method FWN-4604, Determination of % Water by Kad Fischer Titration. The % water results were Cletermined on a Metrohm KFT Titrino Model 795 Titrator (SN ).

Enthalpy Analytical Narrative Summary (continued) Analysis (ph&kft continued) The titrations were performed in a dry methanol reagent.

The 795 KFT uses an internal program and a programmable dosimeter to dispense titrant.

Acetaldehyde, acetoin, diacetyl, and pentanedione were not detected above the lvidl in the laboratory blanks.

10 Enthalpy Analytical Narrative Summary (continued) Analysis (ph&kft continued) The titrations were performed in a dry methanol reagent. Titrant was purchased from Riedel de Haen and had a nominal titrant value of 5 mg water/ml titrant. The 795 KFT uses an internal program and a programmable dosimeter to dispense titrant. Titrant values were read and printed to an Excel spreadsheet. Acetaldehyde, acetoin, diacetyl, and pentanedione were not detected above the lvidl in the laboratory blanks. Formaldehyde was detected below the LOQ in the laboratory blanks. The reported formaldehyde results have been blank-corrected. Nicotine and DEG were not detected above the MDL in the laboratory blanks. The results presented in this report are representative of the samples as provided to the laboratory. EA# Page 10 of 33

General Reporting Notes The following are general reporting notes that are applicable to all Enthalpy Analytical, Inc. data reports, unless specifically noted otherwise.

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.

11 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 Jin 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# Page 11of 33

The LCS is used to assess the control of the laboratory's analytical system. Whenever spikes are prepared for our client projects, two spilces are retained as LCSs.

12 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 spilces 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# Page 12 of 33

13 EA# Page 13 of 33

Chain of Custody Record Page_1 of_1 Special Handling: S~r.

. 't1f =nnalpy An31)'1ical. Inc. AA~ Sampe$ Oi&pos4:.'d ot 1 Mornll Torr: Reoeij:t. AU OtMer Sa: :npll!

.--"""-- - Site Name: Head Office Location: Kenora, Ontario P9N 1A3 4=!e.. l!! > "'

14 Chain of Custody Record Page_1 of_1 Special Handling: S~r.dard Turn Around Time (10 business day~) O Rush Turn Around Time - Date Needed, All TATs Subject to ;>.pp-ov.. 't1f =nnalpy An31)'1ical. Inc. AA~ Sampe$ Oi&pos4:.'d ot 1 Mornll Torr: Reoeij:t. AU OtMer Sa: :npll!'~ Cisposec Qf lllonihs from Receipt. ~=== Project Nurr.ber:..--"""-- - Site Name: Head Office Location: Kenora, Ontario P9N 1A3 4=!e.. l!! > "' s.,.. < ~ en "' c.., 0.. "'.... ::J > a ii: m 0 I- ampe Time Volume T e Matrix 'It 10mL - 'It 'It 'It 'It '~ 10mL d. 10mL ~ 'It April o Iced o Ambient o C D C 0 C Capitola Drive Durham, NC (919) FAX (919) EA# Page 14 ou3

15 EA# Page 15 of 33

$operator: C:\CHEM32\1\DAT A\GC143P096A\042B4801.D \GC\2014\Teller\Quarter2 6/1/2014 8: 17: 1 O AM T05211 4A.$

16 Chromatogram Report Data file: Sample name: Fi le _ Location Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\CHEM32\1\DAT A\GC143P096A\042B4801.D \GC\2014\Teller\Quarter2 6/1/2014 8: 17: 1 O AM T A.M 6/2/ :10:53 PM Teller GC143P096A Kathy Humphries Sample type: Sample Location: Vial 42 Injection volume: Injection: 1 of 1 File_ Version 8 x10 4 of' l~ 2 B. 4.0 :ii u "' 3.5 ~ o_ 3.0 I "' rj1 2.5 ~ c :J 0 u r 1.0..: T1me[minl Signal: FID2 B, N'ame RT min] Area Oil ug/ml Sample_A Units mount Heptadecane ug/ml Diethylene glycol ug/ml EA# Page 16 of 33 Printed: 06/04/ :58:32 Page 9 of 22

$operator: C:\CHEM32\1\DAT A\GC143P096A\043B4901.D \GC\2014\Teller\Quarter2 6/1/2014 8:35:45 AM T05211 4A.$ $0 I "' "'- m rj1 2.5 p c,\.. :J 0 u 2.0 1.5 - -, 1.0 0.5 10 7.2 1.4 7.6 8 6 88 90 9.2 9.4 9.6 9.$

17 Chromatogram Report Data file: Sample name: Fi le _ Location Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\CHEM32\1\DAT A\GC143P096A\043B4901.D \GC\2014\Teller\Quarter2 6/1/2014 8:35:45 AM T A.M 6/2/ :10:53 PM Teller GC143P096A Kathy Humphries Sample type: Sample Location: Vial 43 Injection volume: Injection: 1 of 1 File_ Version 8 x10 4 of' l~ 2 B. 4.0 :ii 3.5 u u "' ro o_ 3.0 I "' "'- m rj1 2.5 p c,\.. :J 0 u , T1me[minl Signal: FID2 B, N'ame RT min] Area Oil ug/ml Sample_A Units mount Heptadecane ug/ml Diethylene glycol ug/ml EA# Page 17 of 33 Printed: 06/04/ :58:32 Page 11of22

$Chromatogram Report Data file: Sample name: C:\CHEM32\1\DAT A\GC143P096A\044B5001.D 0514-132-02-01 File_Location Injection date: Acq.$

18 Chromatogram Report Data file: Sample name: C:\CHEM32\1\DAT A\GC143P096A\044B5001.D File_Location Injection date: Acq. method: Analysis method: Last changed: \GC\2014\Teller\Quarter2 6/1/2014 8:54:43 AM T A.M 6/2/ :10:53 PM Sample type: Location: Injecti on volume: Injection: File_ Version Sample Vial of 1 8 Instrument: Sequence_Name Teller GC143P096A Acq. operator: Kathy Humphries c x10 4 F;{,02 B. N :\' A: ~ u 3_5 (/) 2.5 :J 0 u.. a_ "' 3.0 I ~ )) ro _ g Time (min] Signal: FI02 B, Name Heptadecane Diethylene glycol RT [min] Area Dll ug/ml Sample_A Units mount ug/ml ug/ml EA# Page 18 of 33 Printed: 06/04/ :58:32 Page 13 of 22

$Chromatogram Report Data file: Sample name: C:\CHEM32\1 \DAT A\GC143P096A\045B5101.D 0514-1 32-02-02 File_Location Injection date: Acq.$

19 Chromatogram Report Data file: Sample name: C:\CHEM32\1 \DAT A\GC143P096A\045B5101.D File_Location Injection date: Acq. method: Analysis method: Last changed: \GC\20 14\Teller\Quarter2 6/ 1/2014 9:1 3:37 AM T A.M 6/2/ :10:53 PM Sample type: Location: Injection volume: Injection: File_ Version Sample Vial of 1 8 Instrument: Sequence_Name Teller GC143P096A Acq. operator: Kathy Humphries f;bdz-b X10 4 N : 4.0,..,,_ ro <C. ~ 3.5 ~ a_ "' 3.0 I T1me [min] Signal: FID2 B, Name RT [min] Area Oil ug/ml Sample_A Units mount Heptadecane ug/ml Diethylene glycol ug/ml EA# Page 19 of 33 Printed: 06/04/ :58:32 Page 15 of 22

$Chromatogram Report Data file: C:\CHEM32\1\DAT A\GC143P096A\046B5201.D Sample name: 0514-132-03-01 Fi le _Location Injection date: Acq.$

20 Chromatogram Report Data file: C:\CHEM32\1\DAT A\GC143P096A\046B5201.D Sample name: Fi le _Location Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: \GC\2014\Teller\Quarter2 6/1/2014 9:32:21 AM T052114A.M 6/2/ :10:53 PM Teller GC143P096A Kathy Humphries Sample type: Sample Location: Vial 46 Injection volume: Injection: 1 of 1 File_ Version 8 x10 4 of' l~ 2 B. 4.0 :ii u "' 3.5 ~ o_ 3.0 I "' T1me[minl Signal: FID2 B, N'ame RT min] Area Oil ug/ml Sample_A Units mount Heptadecane ug/ml Diethylene glycol ug/ml EA# Page 20 of 33 Printed: 06/04/ :58:32 Page 17 of 22

$operator: C:\CHEM32\1\DAT A\GC143P096A\047B5301.D \GC\2014\Teller\Quarter2 6/1/2014 9:51:05 AM T052114A.$ M 6/2/2014 12:10:53 PM Teller GC143P096A Kathy Humphries Sample type: Sample Location: Vial 47 Injection volume: 1.000 Injection: 1 of 1 File_ Version 8 c x10 4 of' l~ 2 B. 4.0 :ii u rj1 2.

M 6/2/2014 12:10:53 PM Teller GC143P096A Kathy Humphries Sample type: Sample Location: Vial 47 Injection volume: 1.000 Injection: 1 of 1 File_ Version 8 c x10 4 of' l~ 2 B. 4.0 :ii u rj1 2.

21 Chromatogram Report Data file: Sample name: Fi le _Location Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\CHEM32\1\DAT A\GC143P096A\047B5301.D \GC\2014\Teller\Quarter2 6/1/2014 9:51:05 AM T052114A.M 6/2/ :10:53 PM Teller GC143P096A Kathy Humphries Sample type: Sample Location: Vial 47 Injection volume: Injection: 1 of 1 File_ Version 8 c x10 4 of' l~ 2 B. 4.0 :ii u rj1 2.5 :J 0 u "' 3.5 ~ o_ 3.0 I "' (,- CD T1me[minl Signal: FID2 B, N'ame RT min] Area Oil ug/ml Sample_A Units mount Heptadecane ug/ml Diethylene glycol ug/ml EA# Page 21 of 33 Printed: 06/04/ :58:32 Page 21of22

22 EA# Page 22 of 33

$method: Analysis method: Last changed: C:\CHEM32\ 1\DATA\R060514A\045B480 1.D 0514-132-01-01 Ricky 6/6/2014 6:41:17 AM R060514A.$

23 ~~.-::;,!!E!ll! l'.l lll!l=!!t!!!!!h~ A...L'PV &l,-, c.1 I y t: i c: u I. i ri c:. Data file: Sample name: Description: Instrument: Injection date: Acq. method: Analysis method: Last changed: C:\CHEM32\ 1\DATA\R060514A\045B480 1.D Ricky 6/6/2014 6:41:17 AM R060514A.M 6/9/ :35:41 PM Sequence_Name Location: Injection: Injection_ Volume Acq. operator: Vial45 1 of 1 Kathy Humphries Sample_Multipliers Sample_Dilution Factors N-heptadecane added during an alysis, used for quantitation only RT [min] Type FID2 B, Time [min) Area Amount Name (mg/ml) BB Nicotine EA# Page 23 of 33

24 ~~.-::;,!!E!ll! l'.l lll!l=!!t!!!!!h~ A...L'PV &l,-, c.1 I y t: i c: u I. i ri c:. Data file: Sample name: Description: Instrument: Injection date: Acq. method: Analysis method: Last changed: C:\CHEM32\ 1\DATA\R060514A\046B490 1.D Ricky 6/6/2014 6:58:36 AM R060514A.M 6/9/ :35:41 PM Sequence_Name Location: Injection : Injection_ Volu me Acq. operator: Vial46 1 of 1 Kathy Humphries Sample_Multipliers Sample_Dilution Factors N-heptadecane added during an alysis, used for quantitation only RT [min] Type FID2 B, Time[min] Area Amount Name (mg/ml) BB Nicotine EA# Page 24 of 33

$method: Analysis method: Last changed: C:\CHEM32\ 1\DATA\R060514A\047B500 1.D 0514-132-02-01 Ricky 6/6/2014 7:15:53 AM R060514A.$

25 Sam le Re ort, " '...-, ~~~,!!E!ll!Nlll!!:!!T!!!!H~.A.L'PV &l,-, c.1 I y t: i c: u I. i ri c:. Data file: Sample name: Description: Instrument: Injection date: Acq. method: Analysis method: Last changed: C:\CHEM32\ 1\DATA\R060514A\047B500 1.D Ricky 6/6/2014 7:15:53 AM R060514A.M 6/9/ :35:41 PM Sequence_ Name Location: Injection: Injection_ Volume Acq. operator: Vial47 1 of 1 R A Sample_Multipliers N-heptadecane added during analysis, used for quantitation only D Time[min] 8.0 RT [min] Type FID2 B, Area Amount Name (mg/ml) BB Nicotine EA# Page 25 of 33

26 Sam le Re ort.,....,..,. v., Data fi le: Sample name: Description: Instrument: Injection date: Acq. method: Analysis method: Lasfchanged; C:\CHEM32\ 1\DATA\R060514A\048B5101.D Ricky 6/6/2014 7:33:13 AM R060514A.M 6/9/ :35:41 PM Seq4ence_Name Location: Injection: Injection_ Volume Acq. operator: Vial48 1 of 1 Kathy Humphries N-heptadecane added during an alysis, used for quantitation only Sample_DilutionFactors Time [min) 8.0 RT [min) Type FID2 B, Area Amount Name (mg/ml) BB Nicotine EA# Page 26 of 33

27 ~~.-::;,!!E!ll! l'.l lll!l=!!t!!!!!h~ A...L'PV &l,-, c.1 I y t: i c: u I. i ri c:. Data file: Sample name: Description: Instrument: Injection date: Acq. method: Analysis method: Last changed: C:\CHEM32\ 1\DATA\R060514A\049B530 1.D Ricky 6/6/2014 8:07:37 AM R060514A.M 6/9/ :35:41 PM Sequence_Name Location: Injection : Injection_ Volu me Acq. operator: Vial49 1 of 1 Kathy Humphries Sample_Multipliers Sample_Dilution Factors N-heptadecane added during an alysis, used for quantitation only Time[min) FID2 B, RT [min] Type Area Amount Name (mg/ml) O Nicotine EA# Page 27 of 33

$Sam le Re ort.,....,..,. v., Data fi le: Sample name: Description: Instrument: Injection date: Acq. method: Analysis method: Lasfchanged; C:\CHEM32\ 1\DATA\R060514A\050B5401.$

28 Sam le Re ort.,....,..,. v., Data fi le: Sample name: Description: Instrument: Injection date: Acq. method: Analysis method: Lasfchanged; C:\CHEM32\ 1\DATA\R060514A\050B5401.D Ricky 6/6/2014 8:24:57 AM R060514A.M 6/9/ :35:41 PM Seq4ence_Name Location: Injection: Injection_ Volume Acq. operator: Vial50 1 of 1 Kathy Humphries N-heptadecane added during an alysis, used for quantitation only Sample_Dilution Factors Time [min) 8.0 RT [min) Type FID2 B, Area Amount Name (mg/ml) O Nicotine EA# Page 28 of 33

29 EA# Page 29 of 33

$Chromatogram Report Data file: Sample name: Flle_Location Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\CHEM32\1\DATA\HPLC75PG102 1\029-2201.$ M 5/31/2014 8:56:01 AM Selma HPLC75PG102 1 Wendy Gardow Sample type: Sample Location: Vial 29 Injection volume: 5.

M 5/31/2014 8:56:01 AM Selma HPLC75PG102 1 Wendy Gardow Sample type: Sample Location: Vial 29 Injection volume: 5.

30 Chromatogram Report Data file: Sample name: Flle_Location Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\CHEM32\1\DATA\HPLC75PG102 1\ D \HPLC\2014\Selma\Quarter 2 5/29/2014 4:08:43 AM ELIQUID_BC_EXT.M HPLC75PG096. M 5/31/2014 8:56:01 AM Selma HPLC75PG102 1 Wendy Gardow Sample type: Sample Location: Vial 29 Injection volume: Injection: 1 of 1 File_ Version Name Peak_ Type RT(min) Area Oil ug/ml Sample _Amount Units Aceto in vv ug/ml Formaldehyde vv ug/ml acetaldehyde ug/ml diacetyl ug/ml pentanedione ug/ml Printed: 06/03/ :36:02 Page 2 of 7 Page 30 of 33

$operator: C:\CHEM32\1\DATA\HPLC75PG102 1\030-2301.D 0514-132-02 \HPLC\2014\Selma\Quarter 2 5/29/2014 4:40:06 AM ELIQUID_BC_EXT.M HPLC75PG096.$ $000 1 of 1 220 \fwdf A, Wavel gth=365 nm 210 200 190 180 170 160 150 140 130 120 110 100 90 ~ 80 ~ ff. 70.ff' :ff 60 Q;' ~.fj ~ 50 <; ~ ~ ~ ":' fi...,..., 40 ~ $ ~'II '5' ~.t -~!;' II!$ $20 ::y '?... 1~ ~. i f\ ~ l----<'-~+-~~~~~~~.---'---.--'~~~~~-'--.-~~-'--.$

31 Chromatogram Report Data file: Sample name: Flle_Location Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\CHEM32\1\DATA\HPLC75PG102 1\ D \HPLC\2014\Selma\Quarter 2 5/29/2014 4:40:06 AM ELIQUID_BC_EXT.M HPLC75PG096. M 5/31/2014 8:56:01 AM Selma HPLC75PG102 1 Wendy Gardow Sample type: Location: Injection volume: Injection: File_ Version Sample Vial of \fwdf A, Wavel gth=365 nm ~ 80 ~ ff. 70.ff' :ff 60 Q;' ~.fj ~ 50 <; ~ ~ ~ ":' fi...,..., 40 ~ $ ~'II '5' ~.t -~!;' II! 20 ::y '?... 1~ ~. i f\ ~ l----<'-~+-~~~~~~~.---'---.--'~~~~~-'--.-~~-'--.~~~~~~~~~~~~~~~~~~ ~ Time lminl Name Peak_ Type RT(min) Area Oil ug/ml Sample _Amount Units Aceto in vv ug/ml Formaldehyde VB ug/ml acetaldehyde ug/ml diacetyl ug/ml pentanedione ug/ml Printed: 06/03/ :36:02 Page 3 of 7 Page 31of 33

$operator: C:\CHEM32\1\DATA\HPLC75PG102 1\031-2501.$ M 5/31/2014 8:56:01 AM Selma HPLC75PG102 1 Wendy Gardow Sample type: Location: Injection volume: Injection: File_

M 5/31/2014 8:56:01 AM Selma HPLC75PG102 1 Wendy Gardow Sample type: Location: Injection volume: Injection: File_

$000 1 of 1 220 \fwdf A, W avel gth=365 nm 210 200 190 180 170 160 150 140 130 120 110 100 90 80 70 60 50 40 30 20 10$

32 Chromatogram Report Data file: Sample name: Flle_Location Injection date: Acq. method: Analysis method: Last changed: Instrument: Sequence_Name Acq. operator: C:\CHEM32\1\DATA\HPLC75PG102 1\ D \HPLC\2014\Selma\Quarter 2 5/29/2014 5:42:54 AM ELIQUID_BC_EXT.M HPLC75PG096. M 5/31/2014 8:56:01 AM Selma HPLC75PG102 1 Wendy Gardow Sample type: Location: Injection volume: Injection: File_ Version Sample Vial of \fwdf A, W avel gth=365 nm f\ ~5 Time lminl Name Peak_ Type RT(min) Aceto in BV 7.69 Formaldehyde 8.59 acetaldehyde diacetyl pentanedione Area Oil ug/ml Sample _Amount Units ug/ml ug/ml ug/ml ug/ml ug/ml Printed: 06/03/ :36:02 Page 32 of 33 Page 5 of 7

33 EA# Page 33 of 33

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

Sample RM Analytical Report ( B) HPLC/UV Analysis Acetaldehyde, Acrolein, Crotonaldehyde, Formaldehyde For the benefit of VaporFi, Inc. Sample RM080514 Analytical Report (0814-52B) HPLC/UV Analysis Acetaldehyde, Acrolein, Crotonaldehyde, Formaldehyde GC/MS/MS Analysis 1-Aminonaphthalene, 2-Aminonaphthalene,