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# MPI RESEARC H TSCA-HQ-2004-016 , RCRA-HQ-2004-0016 , TSCA-HQ-2005-500 1 SE P AFluorotelomer-Base d Produc t Characterizatio n Subject : MP I Research Technica l Progres s Repor t

Jun e 26,201 0 t o Jul y23,201 0 1 Introductio n Thi s documen t present s th e progres s of th e technica l wor k fo rcharacterizatio n o f ftuorotelonnerbase d product s an d correspondin g synthesize d o rpurifie d polymers i n suppor t o f th e Biodegradatio n Testin g Supplementa l Environmenta l Projec t ("Biodegradatio n SEP")
. Thi s progres s repor

t i s prepare d pursuan t t o Characterizatio n Laborator yExhibi t A : Scop e o f Work , Sectio n 4f
. Thi s repor

t describe s th e technica l wor k performe d fro m Jun e 26 , 201 0 u p t o th e wee k endin g Jul y23 , 2010 . Th e followin g component s o f th e Wor k Pla n hav e bee n completed : Component s 1 , 2 , 3 , 5 , 6 an d 7 . 

### 2 Progres s Summar y Th e technica l wor k

consiste d o f metho d developmen t outline d i n Componen t 7 ofth e Wor k Plan . LC/MS/M S method s wer e develope d an d draf t method s finalize d fo rth e followin g analytes : 7- 3 Fluorotelome rAcid , 8- 2 Fluorotelome rsaturate d Acid , 8- 2 Fluorotelome runsaturate d Acid , Perfluorooctanoi cAcid , Perfluorononanoi cAcid , Peri'luorodecanoi cAcid an d Perfluoroundecanoi cAcid . GC/M S method s wer e develope d an d draft method s finalize d fo rth e followin g analytes : 6- 2 Fluorotelome rAlcohol , 8- 2 Fluorotelome rAlcohol , 10- 2 Fluorotelome rAlcohol , 8- 2 Fluorotelome r Ethene , 8- 2 Fluorotelome rIodide , 10- 2 Fluorotelome rIodide , Periluoroocty l Iodide , Perfluorodecy l Iodide , 8- 2 Fluorotelome rAcrylate , 7- 2 Fluorotelome riso-ethano l an d PFO Atelome r8- 2 ester . Adraft protoco l fo rth e validatio n of th e GC/M S an d LC/MS/M S method s wa s writte n an d reviewed . Th e protoco l wa s initiate d o n 07/19/2010
. Th e tota l metho d developmen t tim e incurre d fo rth e perio d o f tim e covere d b ythi s repor t wa s 3 1 hours . Th e associate d cos t fo rthi s metho d developmen t wor k i s $775 0 a s identifie d i n Componen t 7 o f th e Wor k Plan . Th e cos t i s base d upo n th e dail yrat e o f $2,000
. Th e tota l cost s associate d wit h th e component s initiate d wit h respec t t o thi s Progres s Repor t ar e $7750.00
. Th e associate d invoic e i s presente d i n Appendi xC
.

MP I Researc h 07/30/201 0 Technica l Progres s Repor t ^^^ ^ ^ ^^" ^THI S DOCUMEN TDOE S NO T CONTAI N CONFIDENTIA L BUSINES S INFORMATIO N (CBI )


### 3 Analysi s b yLC/MS/M S Tw o LC/MS/M S draft method s wer e prepare d an d submitte d fo rQualitycontro l review :
• "Metho d o f Analysi s fo rth e Determinatio n o f 8- 2 Fluorotelome rSaturate d Aci d i n Fluorotelomer-base d Product s an d Correspondin g Synthesize d o rPurifie d Polymers by LC/MS/MS " (V0006601 )
• "Metho d o f Analysi s fo rth e Determinatio n o f Periluorooctanoi cAcid , Periluorononanoi c Acid , Pertluorodecanoi cAcid , Perfluoroundecanoi cAcid , 7- 3 Fluorotelome rAcid , an d 8- 2 Fluorotelome runsaturate d Aci d i n Fluorotelomer-base d Product s an d Correspondin g Synthesize d o rPurifie d Polymers byLC/MS/MS " (V0006602 ) 

### 4 Analysi s b yGC/M S Th e analyse s wer e performe d o n a Agilen t (Formerl yHewlett-Packard ) GC/M S syste m wit h positiv e chemica l ionizatio n usin g heliu m carrie rga s an d methan e reagen t gas . AHP-IM S colum n wa s use d fo rth e developmen t wor k fo rth e followin g analytes : Analvte s 6- 2 Fluorotelome rAlcoho l 8- 2 Fluorotelome rAlcoho l 10- 2 Fluorotelome rAlcoho l 8- 2 Fluorotelome rEthen e 8- 2 Fluorotelome rIodid e 10- 2 Fluorotelome rIodid e Perfluoroocty l Iodid e Perfluorodecy l Iodid e 8- 2 Fluorotelome rAcrylat e 7- 2 Fluorotelome riso-ethano l PFO Atelome r8- 2 este r lUPA C nam e 1 H, 1 H,2H,2H-perfluorooctan-1-o l 1H,1H,2H,2H-perfluorodecan-1-o l 1H,1H,2H,2H-perfluorododecan-1-o l 1H,1H,2H-perfluoro-1-decen e 1H,1H,2H,2H-periluorodecy l iodid e 1 H, 1 H,2H,2H-perfluorododecy l iodid e Perfluoroocty l Iodid e Perfluorodecy l Iodid e 2-propenoicacid , 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10.10 - heptadecafluorodecy l este r 2-nonanol , 3,3,4.4,5,5,6,6,7,7,8,8,9,9,9 - pentadecafluoro Octanoi cacid , pentadecafluoro 3,3,4,4,5,5,6,6,7,7,8,8,9,9,10,10,10 - heptadecafluorodecy l este r CAS # 647-42- 7 678-39- 7 865-86- 1 21652-58- 4 2043-53- 0 2043-54- 1 507-63- 1 423-62- 1 27905-45- 9 24015-83- 6 Not Availabl e
Calibratio n standard s i n MTB E containin g al l analyte s wer e prepared . Th e concentration s fo r eac h analyt e wer e 10 , 20 , 50 , 80 , 100 , 200 , 50 0 an d 100 0 ng/mL
. Linearitywa s achieve d fo r eac h analyt e fro m 1 0 t o 20 0 ng/mL
. 8- 2 Fluorotelome rEthen e wa s analyze d unde rNC I conditio n o n a DB-62 4 colum n (30 m x 0.25m m x1.40p m df)
. Linearitywa s achieve d fro m 1 0 t o 20 0 ng/mL
. Draf t GC/M S method s fo ral l analyte s unde rPC I conditio n an d fo r8- 2 Fluorotelome rEthen e unde rNC I conditio n wer e finalized
.

MP I Researc

h 07/30/201 0 Technica l Progres s Repor t PAGE20F 4THI S DOCUMEN TDOE S NO T CONTAI N CONFIDENTIA L BUSINES S INFORMATIO N (CBI )
Tw o GC/M S draf

t method s wer e prepare d an d submitte d fo rQualitycontro l review :
• "Metho d o f Analysi s fo rth e Determinatio n of Perfluoroocty l Iodide , Perfluorodecy l Iodide , 8- 2 Fluorotelome rIodide , 10- 2 Fluorotelome rIodide , 8- 2 Fluorotelome rAcrylate , 6- 2 Fluorotelome rAlcohol , 7- 2 Fluorotelome riso-ethanol , 8- 2 Fluorotelome rAlcohol , 10- 2 Fluorotelome ralcohol , 8- 2 Fluorotelome rEthen e an d PFO Atelome r8- 2 Este ri n Fluorotelomer-base d Product s an d Correspondin g Synthesize d o rPurifie d Polymers b y GC/PCl/MS " (V0006603 )

• "Metho d o f Analysi s fo rth e Determinatio n o f 8- 2 Fluorotelome rEthen e i n Fluorotelomer base d Product s an d Correspondin g Synthesize d o rPurifie d Polymers byGC/NCI/MS " (V0006604 ) 

### 5 Attachment s 5. 1 Appendi xA : Draf t Method s (LC/MS/MS ) 5. 2 Appendi xB : Draf t Method s an d Ra

wdat a (GC/MS ) 5. 3 Appendi xC : Invoic e 

### 6 Signature s I certifyunde rpenaltyo f lawtha t I hav e examine d an d a m familia rwit h th e informatio n submitte d i n thi s documen t an d al l attachment s an d tha t thi s documen t an d its attachment s wer e prepare d eithe rb ym e personall yo runde rm ydirectio n fo rsupervisio n i n a manne rdesigne d t o ensur e that qualifie d an d knowledgeabl e personne l properl ygathe ran d presen t th e infonnatio n containe d therein . I furthe rcertify , base d o n m ypersona l knowledg e o ro n m yinquir yo f thos e individual s immediatel yresponsibl e fo robtainin g th e information , tha t th e informatio n i s true , accurat e an d complete . I a m aware tha t ther e are significan t penaltie s fo rsubmittin g fals e information , includin g th e possibilityo f fine s an d imprisonmen t fo rknowingl yan d willfull ysubmittin g a materiall yfals e statement .

MP I Researc h 07/30/201 0 Technica l Progres s Repor t ^^^ ^ ^^^" ^THI S DOCUMEN TDOE S NO T CONTAI N CONFIDENTIA L BUSINES S INFORMATIO N (CBI ) 

# OJI? ^ W/ 0 Am ySheehanjuBtud yDirecto r Dat e

MP I Researc h 07/30/201 0 Technica l Progres s Repor t PAG E 4 O F 4