Washwater Analytical Chemistry Review for Cabot Creamery/January 2015/ Stone Environmental, Inc.

Washwater Analytical Chemistry Review for Cabot Creamery

Review of Toxicity Characteristic Leaching Procedure (TCLP) Data generated in December 2014 for the Washwater. Prepared by Kim B. Watson, RQAP-GLP, Stone Environmental Inc.

Executive Summary As part of the Cabot Creamery’s compliance with the conditions of its Indirect Discharge Permit (IDP) for discharging washwater by application on agricultural fields; environmental chemical analyses are performed on the washwater taken directly from the disposal trucks prior to disposal to the agricultural field. A washwater sample was taken from each of the disposal trucks and composited in the field for metals, semivolatile organics, pesticides and herbicides, and one grab sample from the first truck of the day was taken for volatile organics and analyzed for a Toxicity Characteristic Leaching Procedure (TCLP) Test. The TCLP extract generated as a result of processing the liquid and solid washwater is analyzed for the number of parameters for volatile and semivolatile organics, mercury and selected metals by SW846 Methodologies. Only a limited list of compounds makes up the TCLP regulatory analyte list (Attachment A). As required in the VT DEC permit, in addition to reporting the TCLP list of compounds, the full analytical chromatograms and raw data summaries generated at the laboratory were reviewed to determine the presence/absence of a regulatory list of compounds included in the analytical tests which make up the total analysis for these inorganic and organic parameters.

Stone reviewed the organic analysis raw data from Methods 8260 Volatile Organics by Gas Chromatography Mass Spectrometry (GC/MS), Methods 8270 Semivolatile Organics by GC/MS, Method 8081A Pesticides by GC, and Method 8151A Herbicides by GC. In addition, the raw data for metals by Method 6010 was reviewed for the presence/absence of specific metals below the laboratory regulatory reporting limits. Based on review of the raw data which represents a total analysis of the washwater for the above listed parameters, the measurable target organic compounds present in the washwater were 3&4-methyphenol (known as m/p cresol) at 22.9 ppb (ug/L) found in the semi volatile organics (Method 8270) and chloroform at 3.8 ppb found in the volatile organics (Method 8260). Other chromatographic peaks found in the volatile and semi-volatile organic analyses were measured and reported as tentatively identified compounds known

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Washwater Analytical Chemistry Review for Cabot Creamery/January 2015/ Stone Environmental, Inc.

as ethanol, 2-butanol, methylethyl ester acetic acid, n-propyl acetate, methylethyl propanoic acid and butanoic acid in the volatiles analysis and butanoic acid, pentanoic acid, hexanoic acid, octanoic acid, nonanoic acid, n-decanoic acid, dodecanoic acid and n-hexadecanoic acid in the semivolatiles analysis. The tentatively identified compounds estimated concentrations based on peak areas ranged from (15 ppb to 640 ppb). These tentatively identified compounds tend to be breakdown products of CIP detergents and sanitizers (surfactants or disinfectants) and fatty acids found in animals and plants. It should be noted that m/p cresol is regulated under the TCLP and this compound was found well below regulatory limits. Methylphenols are cresols that are used as household cleaners and disinfectants. Barium was the only metal detected at a concentration above the laboratory method detection limit (0.046 mg/L) but well below the TCLP regulatory standard of 100 mg/L. Of the metals reviewed in the raw data, all detections were below the laboratory method detections limits, therefore, were essentially found as a non-detect below the laboratory detection limit well below the TCLP regulatory limit.

Introduction/Objective TCLP analyses are performed on the washwater based on the requirement of the IDP permit and as a result general chemical characteristics of the washwater can be determined from these analyses when reviewed for all method target compounds (see Attachment B). Endyne the laboratory provided the full raw data chromatograms and library searches to determine the following:

1. If other compounds other than the regulatory TCLP compounds analyzed for using these methods were present in measurable concentrations in the total analysis for Method 8260 Volatile Organics by Gas Chromatography Mass Spectrometry (GC/MS), Method 8270 Semivolatile Organics by GC/MS, Method 8081A Pesticides by GC, and Method 8151A Herbicides by GC.

2. Assist the data user in determining the general washwater characteristics as demonstrated from the total analysis for organic compounds.

Results Summary Based on the review of the raw data from the TCLP analyses, which represents a total analysis (target compound lists from the above methods found in Attachment B) of the washwater for the above listed parameters, the measurable target organic compounds present in the washwater were 3&4-methyphenol (known as m/p cresol) at 22.9 ppb (ug/L) found in the semi volatile organics (Method 8270) and chloroform at 3.8 ppb found in the volatile organics (Method 8260) analyses. In addition, to the standard analytes reported in the organic analyses, there were a number of other chromatographic peaks present in the chromatograms for the volatile and semi-volatile organics analyses representing the presence of other compounds. A spectral library search of these chromatographic peaks allows for general chemical characterization of compounds present in the washwater sample for volatiles and semivolatile organics analyses. Based on library searches, the other peaks present represented the breakdown products of the surfactants used in the cleaning

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Washwater Analytical Chemistry Review for Cabot Creamery/January 2015/ Stone Environmental, Inc.

process and saturated fatty acids found in animals and plants. These peaks represent tentatively identified compounds known as ethanol, 2-butanol, methylethyl ester acetic acid, n-propyl acetate, methylethyl propanoic acid and butanoic acid in the volatiles analysis and butanoic acid, pentanoic acid, hexanoic acid, octanoic acid, nonanoic acid, n-decanoic acid, dodecanoic acid and n-hexadecanoic acid in the semivolatiles analysis. Only peaks greater than 10 percent of the internal standard were searched representing the approximate detection limit for the analytical method, and reported as additional materials found in Attachment B. The approximate concentrations of these compounds were found to be at 15 ppb to 640 ppb. These tentative identifications are tentative at best since they are not supported with analytical standards.

It should be noted that m/p cresol and chloroform are regulated under the TCLP and these compounds were found well below regulatory limits. Chloroform is a known by-product of chlorination and 3/4 methylphenol are cresols that are used as household cleaners and disinfectants.

Barium was the only metal detected at a concentration above the laboratory detection limit (0.0462 mg/L) but well below the TCLP regulatory standard of 100 mg/L. Of the metals reviewed in the raw data, all detections were below the laboratory method detections limits, therefore, were essentially found as a non-detect below the laboratory detection limit well below the TCLP regulatory limit.

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ATTACHMENT A

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ATTACHMENT B

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Laboratory Report

Cabot Creamery TruckPROJECT:

DATE RECEIVED:

WORK ORDER:

DATE REPORTED:

070157

The Johnson Company

100 State Street Suite 600

Montpelier, VT 05602

Atten: Jim Bowes SAMPLER:

January 22, 2015

1412-24917

Jeremy Matt

December 03, 2014

Enclosed please find the results of the analyses performed for the samples referenced on the attached chain of custody. All required method quality control elements including instrument calibration were performed in accordance with method requirements and determined to be acceptable unless otherwise noted.

The column labeled Lab/Tech in the accompanying report denotes the laboratory facility where the testing was performed and the technician who conducted the assay. A "W" designates the Williston, VT lab under NELAC certification ELAP 11263; "R" designates the Lebanon, NH facility under certification NH 2037 and “N” the Plattsburgh, NY lab under certification ELAP 11892. “Sub” indicates the testing was performed by a subcontracted laboratory. The accreditation status of the subcontracted lab is referenced in the corresponding NELAC and Qual fields.

The NELAC column also denotes the accreditation status of each laboratory for each reported parameter. “A” indicates the referenced laboratory is NELAC accredited for the parameter reported. “N” indicates the laboratory is not accredited. “U” indicates that NELAC does not offer accreditation for that parameter in that specific matrix. Test results denoted with an “A” meet all National Environmental Laboratory Accreditation Program requirements except where denoted by pertinent data qualifiers. Test results are representative of the samples as they were received at the laboratory

Endyne, Inc. warrants, to the best of its knowledge and belief, the accuracy of the analytical

test results contained in this report, but makes no other warranty, expressed or implied, especially no warranties of merchantability or fitness for a particular purpose.

Page 1 of 3

Reviewed by:

Harry B. Locker, Ph.D.

Laboratory Director

ELAP 11263

160 James Brown Dr., Williston, VT 05495

Ph 802-879-4333 Fax 802-879-7103

www.endynelabs.com

NH2037

56 Etna Road, Lebanon, NH 03766

Ph 603-678-4891 Fax 603-678-4893Page 7 of 60

Laboratory Report

The Johnson Company

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CLIENT:PROJECT: Cabot Creamery Truck

WORK ORDER:DATE RECEIVED

1412-2491712/03/2014

DATE REPORTED: 01/22/2015

001 Date Sampled: 12/3/14Site: Truck Composite Time: 5:30

Analysis Date/TimeMethodParameter Result NELACLab/TechUnits Qual.

Completed 12/8/14 RGTW ATCLP Extract-SVOA/Metals EPA 1311

< 0.20 mg/L 12/16/14 MGTW AArsenic, Total TCLP EPA 6010C

< 0.20 mg/L 12/16/14 MGTW ABarium, Total TCLP EPA 6010C

< 0.020 mg/L 12/16/14 MGTW ACadmium, Total TCLP EPA 6010C

< 0.05 mg/L 12/16/14 MGTW AChromium, Total TCLP EPA 6010C

< 0.20 mg/L 12/16/14 MGTW ALead, Total TCLP EPA 6010C

< 0.010 mg/L 12/17/14 EERW AMercury, Total TCLP EPA 7470

< 0.50 mg/L 12/17/14 CMW ASelenium, Total TCLP EPA 7010

< 0.20 mg/L 12/16/14 MGTW ASilver, Total TCLP EPA 6010C

TCLP PESTICIDES

Completed 12/10/14 FAAW ALiq/Liq Solvent Extraction EPA 3510C

< 0.0020 mg/L 12/10/14 MDPW ALindane, TCLP EPA 8081A

< 0.0020 mg/L 12/10/14 MDPW AHeptachlor, TCLP EPA 8081A

< 0.0020 mg/L 12/10/14 MDPW AHeptachlor Epoxide, TCLP EPA 8081A

< 0.0020 mg/L 12/10/14 MDPW AEndrin, TCLP EPA 8081A

< 0.0040 mg/L 12/10/14 MDPW AMethoxychlor, TCLP EPA 8081A

< 0.010 mg/L 12/10/14 MDPW AChlordane, TCLP EPA 8081A

< 0.010 mg/L 12/10/14 MDPW AToxaphene, TCLP EPA 8081A

59 % 12/10/14 MDPW ASurrogate-TCMX EPA 8081A

73 % 12/10/14 MDPW ASurrogate-DCB EPA 8081A

TCLP HERBICIDES

Completed 12/15/14 FAAW ALiq/Liq Solvent Extraction EPA 3510C

< 0.25 mg/L 12/16/14 MDPW A2,4-D, TCLP EPA 8151A

< 0.10 mg/L 12/16/14 MDPW A2,4,5-TP, TCLP EPA 8151A

89 % 12/16/14 MDPW ASurrogate-DCAA EPA 8151A

TCLP SEMI-VOLATILES

Completed 12/10/14 FAAW ALiq/Liq Solvent Extraction EPA 3510C

< 0.2 mg/L 12/23/14 EEPW APyridine, TCLP EPA 8270C

< 0.05 mg/L 12/23/14 EEPW AHexachloroethane, TCLP EPA 8270C

< 0.05 mg/L 12/23/14 EEPW ANitrobenzene, TCLP EPA 8270C

< 0.05 mg/L 12/23/14 EEPW AHexachlorobutadiene, TCLP EPA 8270C

< 0.05 mg/L 12/23/14 EEPW A2,4-Dinitrotoluene, TCLP EPA 8270C

< 0.05 mg/L 12/23/14 EEPW AHexachlorobenzene, TCLP EPA 8270C

< 0.1 mg/L 12/23/14 EEPW UCresols, Total TCLP EPA 8270C

< 0.1 mg/L 12/23/14 EEPW A2,4,5-Trichlorophenol, TCLP EPA 8270C

< 0.1 mg/L 12/23/14 EEPW A2,4,6-Trichlorophenol, TCLP EPA 8270C

< 0.2 mg/L 12/23/14 EEPW APentachlorophenol, TCLP EPA 8270C

72 % 12/23/14 EEPW AB/N Surr.1 Nitrobenzene-d5 EPA 8270C

74 % 12/23/14 EEPW AB/N Surr.2 2-Fluorobiphenyl EPA 8270C

97 % 12/23/14 EEPW AB/N Surr.3 Terphenyl-d14 EPA 8270C

32 % 12/23/14 EEPW AAcid Surr.1 2-Fluorophenol EPA 8270C

27 % 12/23/14 EEPW AAcid Surr.2 Phenol-d8 EPA 8270C

84 % 12/23/14 EEPW AAcid Surr.3 Tribromophenol EPA 8270C

002 Date Sampled: 12/3/14Site: Truck Grab Time: 5:00

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Laboratory Report

The Johnson Company

Page 3 of 3

CLIENT:PROJECT: Cabot Creamery Truck

WORK ORDER:DATE RECEIVED

1412-2491712/03/2014

DATE REPORTED: 01/22/2015

002 Date Sampled: 12/3/14Site: Truck Grab Time: 5:00

Analysis Date/TimeMethodParameter Result NELACLab/TechUnits Qual.

Completed 12/15/14 RGTW ATCLP Extract-VOA ZHE EPA 1311

TCLP VOLATILES

< 0.020 mg/L 12/16/14 SJMW AVinyl chloride, TCLP EPA 8260B

< 0.010 mg/L 12/16/14 SJMW A1,1-Dichloroethene, TCLP EPA 8260B

< 0.10 mg/L 12/16/14 SJMW A2-Butanone (MEK), TCLP EPA 8260B

< 0.010 mg/L 12/16/14 SJMW AChloroform, TCLP EPA 8260B

< 0.010 mg/L 12/16/14 SJMW ACarbon tetrachloride, TCLP EPA 8260B

< 0.010 mg/L 12/16/14 SJMW ABenzene, TCLP EPA 8260B

< 0.010 mg/L 12/16/14 SJMW A1,2-Dichloroethane, TCLP EPA 8260B

< 0.010 mg/L 12/16/14 SJMW ATrichloroethene, TCLP EPA 8260B

< 0.010 mg/L 12/16/14 SJMW ATetrachloroethene, TCLP EPA 8260B

< 0.010 mg/L 12/16/14 SJMW AChlorobenzene, TCLP EPA 8260B

< 0.010 mg/L 12/16/14 SJMW A1,4-Dichlorobenzene, TCLP EPA 8260B

112 % 12/16/14 SJMW ASurr. 1 (Dibromofluoromethane) EPA 8260B

98 % 12/16/14 SJMW ASurr. 2 (Toluene d8) EPA 8260B

93 % 12/16/14 SJMW ASurr. 3 (4-Bromofluorobenzene) EPA 8260B

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Work Order: 1412-24917Site: Truck Composite Date Sampled: 12‐3‐2014 5:30

CompoundLab QL    

mg/L

Lab MDL 

ug/L

Lab QL 

ug/L

VGES 

ug/L

Reported 

TCLP Results 

ug/L

Actual Results 

Calculated 

from Raw data 

ug/LU=ND at 

stated QL

Detected 

below 

VGES

Arsenic 0.200 6.7 200 10 <200 <MDL U *Barium 0.020 0.36 20 2000 <200 46.2 YCadmium 0.020 0.42 20 5 <20 <MDL U YChromium 0.050 0.44 50 100 <50 <MDL U YLead 0.200 3.0 200 15 <200 <MDL U YSelenium 0.500 0.324 500 50 <500 <MDL U YSilver 0.200 2.3 200 100 <200 <MDL U YMercury 0.010 0.031 10.0 2 <10 <MDL U YNote: Secondary standard for silver only.

NA=Not available

*Although arsenic was not detected (ND) in the analytical run, due to the 10 fold dilution performed during sample prep,

the adjusted detection limit was above the action limit.

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File :C:\msdchem\1\12161426.DOperator : Acquired : 16 Dec 2014 8:42 pm using AcqMethod AQ-8260.MInstrument : JulioSample Name: 1412-24917-002 10% Misc Info : Vial Number: 10

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Library Search Compound Report

Data Path : C:\msdchem\1\ Data File : 12161426.D Acq On : 16 Dec 2014 8:42 pm Operator : Sample : 1412-24917-002 10% Misc : ALS Vial : 10 Sample Multiplier: 1

Quant Method : C:\msdchem\1\METHODS\8260full-121014.M Quant Title : 8260c

TIC Library : C:\Database\NIST08.L TIC Integration Parameters: rteint.p

********************************************************************* Peak Number 1 Acetic acid, bromochloro- Concentration Rank 6

R.T. EstConc Area Relative to ISTD R.T. --------------------------------------------------------------------- 4.420 1.97 ug/L 47473 Pentafluorobenzene 8.036

Hit# of 5 Tentative ID MW MolForm CAS# Qual --------------------------------------------------------------------- 1 Acetic acid, bromochloro- 172 C2H2BrClO2 005589-96-8 9 2 Propanoic acid, 2-chloro-, ethyl... 136 C5H9ClO2 000535-13-7 9 3 Ethanol, 2-[2-(2-chloroethoxy)et... 244 C12H17ClO3 1000268-11-3 7 4 Dimethyl Sulfoxide 78 C2H6OS 000067-68-5 5 5 Dimethyl Sulfoxide 78 C2H6OS 000067-68-5 5

********************************************************************* Peak Number 2 Ethanol Concentration Rank 3

R.T. EstConc Area Relative to ISTD R.T. --------------------------------------------------------------------- 5.248 8.77 ug/L 211080 Pentafluorobenzene 8.036

Hit# of 5 Tentative ID MW MolForm CAS# Qual --------------------------------------------------------------------- 1 Ethanol 46 C2H6O 000064-17-5 74 2 Ethanol 46 C2H6O 000064-17-5 9 3 Ethanol 46 C2H6O 000064-17-5 9 4 Dimethyl ether 46 C2H6O 000115-10-6 9 5 Dimethyl ether 46 C2H6O 000115-10-6 4

********************************************************************* Peak Number 3 2-Butanol, (.+/-.)- Concentration Rank 9

R.T. EstConc Area Relative to ISTD R.T. --------------------------------------------------------------------- 7.681 1.54 ug/L 37074 Pentafluorobenzene 8.036

Hit# of 5 Tentative ID MW MolForm CAS# Qual --------------------------------------------------------------------- 1 2-Butanol, (.+/-.)- 74 C4H10O 015892-23-6 83 2 2-Butanol 74 C4H10O 000078-92-2 83 3 2-Butanol, (R)- 74 C4H10O 014898-79-4 83 4 2-Butanol 74 C4H10O 000078-92-2 78 5 2-Butanol 74 C4H10O 000078-92-2 74

********************************************************************* Peak Number 4 Acetic acid, 1-methylethyl ... Concentration Rank 1

R.T. EstConc Area Relative to ISTD R.T. --------------------------------------------------------------------- 8.440 18.15 ug/L 437006 Pentafluorobenzene 8.036

2 of 22Page 24 of 60

Hit# of 5 Tentative ID MW MolForm CAS# Qual --------------------------------------------------------------------- 1 Acetic acid, 1-methylethyl ester 102 C5H10O2 000108-21-4 74 2 Acetic acid, 1-methylethyl ester 102 C5H10O2 000108-21-4 64 3 Acetic acid, 1-methylethyl ester 102 C5H10O2 000108-21-4 43 4 Acetic acid, 1-methylethyl ester 102 C5H10O2 000108-21-4 9 5 o-Ethylhydroxylamine 61 C2H7NO 1000322-42-5 4

********************************************************************* Peak Number 5 n-Propyl acetate Concentration Rank 2

R.T. EstConc Area Relative to ISTD R.T. --------------------------------------------------------------------- 9.445 16.01 ug/L 287542 1,4-Difluorobenzene 8.854

Hit# of 5 Tentative ID MW MolForm CAS# Qual --------------------------------------------------------------------- 1 n-Propyl acetate 102 C5H10O2 000109-60-4 74 2 n-Propyl acetate 102 C5H10O2 000109-60-4 74 3 n-Propyl acetate 102 C5H10O2 000109-60-4 9 4 1-Butanamine 73 C4H11N 000109-73-9 4 5 1-Butanamine 73 C4H11N 000109-73-9 4

********************************************************************* Peak Number 6 Propanoic acid, 1-methyleth... Concentration Rank 8

R.T. EstConc Area Relative to ISTD R.T. --------------------------------------------------------------------- 10.086 1.64 ug/L 29406 1,4-Difluorobenzene 8.854

Hit# of 5 Tentative ID MW MolForm CAS# Qual --------------------------------------------------------------------- 1 Propanoic acid, 1-methylethyl ester 116 C6H12O2 000637-78-5 64 2 Propanoic acid, 1-methylethyl ester 116 C6H12O2 000637-78-5 64 3 Propanoic acid, 1-methylethyl ester 116 C6H12O2 000637-78-5 42 4 Propionic acid, 4-hydroxy-3-hexy... 174 C9H18O3 1000151-16-9 33 5 o-Isopropylhydroxylamine 75 C3H9NO 1000322-42-6 9

********************************************************************* Peak Number 7 Butanoic acid, 1-methylethy... Concentration Rank 5

R.T. EstConc Area Relative to ISTD R.T. --------------------------------------------------------------------- 11.603 2.50 ug/L 43704 Chlorobenzene-d5 12.076

Hit# of 5 Tentative ID MW MolForm CAS# Qual --------------------------------------------------------------------- 1 Butanoic acid, 1-methylethyl ester 130 C7H14O2 000638-11-9 39 2 Propyl nitrite 89 C3H7NO2 000543-67-9 9 3 Butanoic acid, pentyl ester 158 C9H18O2 000540-18-1 9 4 N-Hydroxymethylacetamide 89 C3H7NO2 000625-51-4 9 5 Azetidine, 2-methyl- 71 C4H9N 019812-49-8 4

********************************************************************* Peak Number 8 7-Hydroxy-7,8,9,10-tetramet... Concentration Rank 4

R.T. EstConc Area Relative to ISTD R.T. --------------------------------------------------------------------- 23.200 3.69 ug/L 52502 1,4-Dichlorobenzene-d4 14.805

Hit# of 5 Tentative ID MW MolForm CAS# Qual --------------------------------------------------------------------- 1 7-Hydroxy-7,8,9,10-tetramethyl-7... 252 C18H20O 1000110-34-9 9 2 Cyclopenteno[4.3-b]tetrahydrofur... 358 C19H18O5S 1000211-22-7 9 3 Indole-2-one, 2,3-dihydro-N-hydr... 207 C11H13NO3 1000129-52-1 9

3 of 22Page 25 of 60

4 2-Ethylacridine 207 C15H13N 055751-83-2 7 5 Pyrido[2,3-d]pyrimidine, 4-phenyl- 207 C13H9N3 028732-75-4 5

********************************************************************* Peak Number 9 2-Ethylacridine Concentration Rank 7

R.T. EstConc Area Relative to ISTD R.T. --------------------------------------------------------------------- 23.545 1.92 ug/L 27351 1,4-Dichlorobenzene-d4 14.805

Hit# of 5 Tentative ID MW MolForm CAS# Qual --------------------------------------------------------------------- 1 2-Ethylacridine 207 C15H13N 055751-83-2 9 2 2,3,4-Trimethoxyphenylacetonitrile 207 C11H13NO3 068913-85-9 9 3 1H-Isoindole-1,3(2H)-dione, 5-ni... 192 C8H4N2O4 000089-40-7 7 4 Phenanthrene, tetradecahydro- 192 C14H24 005743-97-5 7 5 1,4-Phthalazinedione, 2,3-dihydr... 207 C8H5N3O4 003682-19-7 5

8270D-122314.M Mon Mar 02 09:33:09 2015 5975

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TIC: 12161426.D\data.ms1412-24917-002 10%

Peak # Ret Time Type Width Area Start Time End Time 1 4.420 rBV 0.266 47473 4.361 4.627 2 5.248 rVB 0.532 211080 5.198 5.730 3 6.115 rVB 0.168 99471 6.065 6.233 4 7.681 rVB 0.207 37074 7.632 7.839 5 8.036 rVB 0.217 1203811 7.987 8.204 6 8.440 rBV 0.177 437006 8.391 8.568 7 8.854 rBV 0.118 898171 8.795 8.913 8 9.445 rVB 0.168 287542 9.386 9.553 9 10.086 rBV 0.138 29406 10.036 10.174 10 10.450 rBV 0.108 1274172 10.391 10.499 11 11.603 rVB 0.148 43704 11.554 11.701 12 12.066 rBV 0.266 875378 12.017 12.283 13 13.406 rBV 0.286 509280 13.357 13.643 14 14.805 rBV 0.246 710780 14.756 15.002 15 23.200 rBV 0.759 52502 22.471 23.230 16 23.545 rVV 0.670 27351 23.230 23.900

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(Text File) Scan 288 (6.115 min): 12161426.D\data.ms

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1 R 927 956R 79.1P Acetic acid, hydrazide2 M 900 915R 79.1P Acetic acid, hydrazide3 R 883 899R 17.1P Acetic acid, methyl ester4 M 866 881R 17.1P Acetic acid, methyl ester5 R 866 880R 17.1P Acetic acid, methyl ester6 R 770 818R 1.05P 2-Propanone, 1-hydroxy-7 R 770 784R 1.05P 1-Propanol, 2-methyl-8 M 768 808R 0.97P 1.2-diacetylhydrazine9 M 765 812R 1.05P 2-Propanone, 1-hydroxy-

10 R 754 773R 1.05P 1-Propanol, 2-methyl-11 R 736 750R 1.05P 1-Propanol, 2-methyl-12 M 731 743R 0.23P 4-Aminoisoxazolidin-3-one13 R 712 748R 0.97P 1.2-diacetylhydrazine14 R 711 725R 1.05P 2-Propanone, 1-hydroxy-15 M 707 719R 1.05P 1-Propanol, 2-methyl-16 R 702 717R 0.06P Diacetamide17 R 699 711R 0.05P Cycloserine18 M 695 807R 0.05P Acetohydroxamic Acid19 M 691 703R 0.04P 1,2-Ethanediol, monoacetate20 M 688 717R 0.03P 1,2,3-Propanetriol, monoacetate21 M 679 830R 0.02P Acetic anhydride22 M 676 729R 0.02P Methyl(methyl-4-deoxyβl-threo-hex-4-enopyranosid)uronate23 R 674 709R 0.02P N-Nitrosodimethylamine24 R 671 682R 0.01P 1,2-Epoxy-3-propyl acetate25 R 671 681R 0.04P 1,2-Ethanediol, monoacetate26 R 670 680R 0.97P 1.2-diacetylhydrazine27 R 668 680R 0.04P 1,2-Ethanediol, monoacetate28 R 659 668R 0.01P Butanoic acid, 3-oxo-, methyl ester29 M 658 669R 0.01P Urea, N-ethyl-N-nitroso-30 M 648 662R 0.06P Diacetamide31 M 646 657R 0.00P Urea, methyl-32 R 646 656R 0.01P Butanoic acid, 3-oxo-, methyl ester33 M 643 654R 0.00P 2(3H)-Furanone, dihydro-4-hydroxy-34 R 639 654R 0.02P N-Nitrosodimethylamine35 M 633 646R 0.00P Oxalic acid, ethyl propyl ester36 R 633 644R 0.00P Aminoguanidine37 M 631 740R 0.00P Propanoic acid, 2-oxo-38 M 630 645R 0.00P Propanoic acid, 2-oxo-, methyl ester39 R 628 728R 0.00P Dimethadione40 M 626 762R 0.00P 1-Isopropyl-3,3-bis(trifluoromethyl)diaziridine41 M 626 635R 0.00P N-Acetylcycloserine42 M 623 634R 0.00P O-Methylisourea43 M 621 741R 0.00P Diacetyl sulphide44 M 616 627R 0.00P o-Methylisourea hydrogen sulfate45 M 613 623R 0.00P Aminoguanidine46 R 608 618R 0.01P Urea, N-ethyl-N-nitroso-47 R 604 642R 0.05P Acetohydroxamic Acid48 M 604 616R 0.00P Acetic acid, (acetyloxy)-49 M 603 617R 0.00P Hydrazinecarboximidamide, nitrate50 M 600 721R 0.00P Butanenitrile, 2,3-dioxo-, dioxime, o,o'-diacetyl-51 M 599 714R 0.00P Pyrimidine-2,4(1H,3H)-dione, 5-amino-6-nitroso-52 R 596 628R 0.03P 1,2,3-Propanetriol, monoacetate53 M 595 604R 0.05P Cycloserine54 R 594 609R 0.00P Propanoic acid, 2-oxo-, ethyl ester55 R 592 625R 0.02P N-Nitrosodimethylamine56 M 592 607R 0.00P Acetamide, N-(aminocarbonyl)-57 M 590 681R 0.00P Ethanimidic acid, ethyl ester58 M 590 599R 0.00P 1,2,3-Propanetriol, 1-acetate59 R 584 599R 0.01P Butanoic acid, 3-oxo-, methyl ester60 R 584 593R 0.00P Butanoic acid, methyl ester61 M 583 618R 0.00P Formic acid, ethenyl ester62 M 583 592R 0.00P Butanoic acid, methyl ester63 M 583 592R 0.00P Propanoic acid, 3-hydroxy-, methyl ester64 ni 582 591R 0.00P Tetramethylammonium acetate

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Library Searched : C:\Database\NIST08.LQuality : 9ID : Acetic acid, hydrazide

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Abundance Scan 288 (6.115 min): 12161426.D\data.ms43

74

59

207

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Abundance #774: Acetic acid, hydrazide32

43

15

745926

NH

O

NH2

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File :C:\msdchem\1\DATA\Dec2014\12231420.DOperator : Acquired : 23 Dec 2014 6:02 pm using AcqMethod AQ-8270D.MInstrument : SVOC #1Sample Name: 1412-24917-001 Misc Info : 0.10L 12/10/14 Vial Number: 17

4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00

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Abundance TIC: 12231420.D\data.ms

3.885

4.743

4.813

5.597

5.639

5.924

6.302

6.441

6.931

7.074

7.128

7.381 7.473

8.062 8.173

8.836

9.061

9.251

9.609

9.988

10.293

10.835

11.948

13.462

16.288

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Library Search Compound Report

Data Path : C:\msdchem\1\DATA\Dec2014\ Data File : 12231420.D Acq On : 23 Dec 2014 6:02 pm Operator : Sample : 1412-24917-001 Misc : 0.10L 12/10/14 ALS Vial : 17 Sample Multiplier: 1

Quant Method : C:\msdchem\1\METHODS\8270D-122314.M Quant Title : SW 8270D Calibration

TIC Library : C:\Database\NIST08.L TIC Integration Parameters: rteint.p

********************************************************************* Peak Number 1 Butanoic acid Concentration Rank 6

R.T. EstConc Area Relative to ISTD R.T. --------------------------------------------------------------------- 3.886 4.98 ug 136000 1,4-Dichlorobenzene d-4 (I.S.) 5.920

Hit# of 5 Tentative ID MW MolForm CAS# Qual --------------------------------------------------------------------- 1 Butanoic acid 88 C4H8O2 000107-92-6 90 2 Butanoic acid 88 C4H8O2 000107-92-6 90 3 2-Butanol, 3-methyl- 88 C5H12O 000598-75-4 7 4 Propanal, 3-methoxy- 88 C4H8O2 002806-84-0 4 5 Propane, 2-ethoxy- 88 C5H12O 000625-54-7 4

********************************************************************* Peak Number 2 Pentanoic acid Concentration Rank 4

R.T. EstConc Area Relative to ISTD R.T. --------------------------------------------------------------------- 4.815 9.79 ug 267414 1,4-Dichlorobenzene d-4 (I.S.) 5.920

Hit# of 5 Tentative ID MW MolForm CAS# Qual --------------------------------------------------------------------- 1 Pentanoic acid 102 C5H10O2 000109-52-4 64 2 Pentanoic acid 102 C5H10O2 000109-52-4 64 3 Pentanoic acid 102 C5H10O2 000109-52-4 9 4 Butanoic acid 88 C4H8O2 000107-92-6 9 5 Propanamide 73 C3H7NO 000079-05-0 5

********************************************************************* Peak Number 3 Hexanoic acid Concentration Rank 3

R.T. EstConc Area Relative to ISTD R.T. --------------------------------------------------------------------- 5.640 13.70 ug 374162 1,4-Dichlorobenzene d-4 (I.S.) 5.920

Hit# of 5 Tentative ID MW MolForm CAS# Qual --------------------------------------------------------------------- 1 Hexanoic acid 116 C6H12O2 000142-62-1 83 2 Hexanoic acid 116 C6H12O2 000142-62-1 83 3 Hexanoic acid 116 C6H12O2 000142-62-1 83 4 Hexanoic acid 116 C6H12O2 000142-62-1 83 5 Propanedioic acid, propyl- 146 C6H10O4 000616-62-6 56

********************************************************************* Peak Number 4 Octanoic Acid Concentration Rank 2

R.T. EstConc Area Relative to ISTD R.T. --------------------------------------------------------------------- 6.932 47.73 ug 1801390 Naphthalene-d8 (I.S) 7.124

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Hit# of 5 Tentative ID MW MolForm CAS# Qual --------------------------------------------------------------------- 1 Octanoic Acid 144 C8H16O2 000124-07-2 90 2 Octanoic Acid 144 C8H16O2 000124-07-2 90 3 Octanoic Acid 144 C8H16O2 000124-07-2 86 4 Hexanoic acid 116 C6H12O2 000142-62-1 64 5 Hexanoic acid 116 C6H12O2 000142-62-1 53

********************************************************************* Peak Number 5 Octanoic Acid Concentration Rank 8

R.T. EstConc Area Relative to ISTD R.T. --------------------------------------------------------------------- 7.471 2.92 ug 110229 Naphthalene-d8 (I.S) 7.124

Hit# of 5 Tentative ID MW MolForm CAS# Qual --------------------------------------------------------------------- 1 Octanoic Acid 144 C8H16O2 000124-07-2 53 2 Heptanoic acid 130 C7H14O2 000111-14-8 50 3 Nonanoic acid 158 C9H18O2 000112-05-0 50 4 Heptanoic acid 130 C7H14O2 000111-14-8 47 5 Octanoic Acid 144 C8H16O2 000124-07-2 42

********************************************************************* Peak Number 6 n-Decanoic acid Concentration Rank 1

R.T. EstConc Area Relative to ISTD R.T. --------------------------------------------------------------------- 8.063 63.67 ug 2594400 Acenaphthene-d10 (I.S.) 8.836

Hit# of 5 Tentative ID MW MolForm CAS# Qual --------------------------------------------------------------------- 1 n-Decanoic acid 172 C10H20O2 000334-48-5 98 2 n-Decanoic acid 172 C10H20O2 000334-48-5 91 3 n-Decanoic acid 172 C10H20O2 000334-48-5 90 4 n-Decanoic acid 172 C10H20O2 000334-48-5 76 5 n-Decanoic acid 172 C10H20O2 000334-48-5 72

********************************************************************* Peak Number 7 Dodecanoic acid Concentration Rank 5

R.T. EstConc Area Relative to ISTD R.T. --------------------------------------------------------------------- 9.059 6.28 ug 255910 Acenaphthene-d10 (I.S.) 8.836

Hit# of 5 Tentative ID MW MolForm CAS# Qual --------------------------------------------------------------------- 1 Dodecanoic acid 200 C12H24O2 000143-07-7 99 2 Dodecanoic acid 200 C12H24O2 000143-07-7 93 3 Dodecanoic acid 200 C12H24O2 000143-07-7 91 4 Dodecanoic acid 200 C12H24O2 000143-07-7 90 5 Undecanoic acid 186 C11H22O2 000112-37-8 80

********************************************************************* Peak Number 8 Tetradecanoic acid Concentration Rank 9

R.T. EstConc Area Relative to ISTD R.T. --------------------------------------------------------------------- 9.983 1.70 ug 67546 Phenanthrene-d10 (I.S.) 10.289

Hit# of 5 Tentative ID MW MolForm CAS# Qual --------------------------------------------------------------------- 1 Tetradecanoic acid 228 C14H28O2 000544-63-8 98 2 Tetradecanoic acid 228 C14H28O2 000544-63-8 97 3 Tetradecanoic acid 228 C14H28O2 000544-63-8 94

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4 n-Hexadecanoic acid 256 C16H32O2 000057-10-3 87 5 Tridecanoic acid 214 C13H26O2 000638-53-9 72

********************************************************************* Peak Number 9 n-Hexadecanoic acid Concentration Rank 7

R.T. EstConc Area Relative to ISTD R.T. --------------------------------------------------------------------- 10.834 4.25 ug 169268 Phenanthrene-d10 (I.S.) 10.289

Hit# of 5 Tentative ID MW MolForm CAS# Qual --------------------------------------------------------------------- 1 n-Hexadecanoic acid 256 C16H32O2 000057-10-3 99 2 n-Hexadecanoic acid 256 C16H32O2 000057-10-3 93 3 Tridecanoic acid 214 C13H26O2 000638-53-9 91 4 Pentadecanoic acid 242 C15H30O2 001002-84-2 90 5 n-Hexadecanoic acid 256 C16H32O2 000057-10-3 87

8270D-122314.M Mon Mar 02 09:47:41 2015 5975

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