1 Responses to EPA Review of Fluoropolymers Incineration ECA Final Study Report

The	text	below	responds	to	each of	the	Questions	on	the	Final	S tudy	Report	for	Fluoropolymer

Incineration	ECA	Testing	sent	by e‐mail	on	May	20,	2013	from	Jo e	Avcin	of	EPA	to	Philip	Taylor.

Both	Phase	I	and	Phase	II	testing	described	in	the	Final	Study Report	were	performed	in	accordance

with	the	requirements	of	the	Enf orceable	Consent Agreement	(ECA )	and	TSCA	GLPs	as	embodied	in

the	EPA‐approved	Quality	Assuranc e	Project	Plans	(QAPPs).		The project	team	established	and

executed	a	quality	management	system	to	assure	conformance	with the	EPA‐approved	QAPPs	and

documented	such	conformance	in	t he	Final	Study	Report	submitted October	30,	2009.

Area #1

– Preparation of Composite #3

The ECA test protocol stipulates that the four fluoropolymer test substance composites will consist of

the 17 components listed in Table 1 below. Composite #1 shall be representative of a dry non

‐ melt resin

and will contain compound numbers 1, 3, and 13. Composite #2 shall be representative of a dry melt

resin and will contain compound numbers 2, 3, 4, 5, 6, and 12. Composite #3 shall be representative of

a fluoroelastomer (a dry non

‐ melt gum) and will contain compound numbers 4, 7, 8, 9, 10, 11, 15, 16,

and 17. Composite #4 shall be representative of an aqueous dispersion and will contain compound

numbers 1, 2, 3, 4, and 14. However, the documented composition of Composite #3 does not seem to

comply with the stipulations of the ECA test protocol.

According to the Phase II composite preparation report, Composite 3 does not appear to have been

prepared with all specified materials. The composite preparation data logs indicated that compound 4

and 7 were not included in the composition of the composite. Upon further review, it appears that

Dyneon, LLC was responsible for providing compound 4 for Composite 2 and 4. However, it is unclear

whether the company was also responsible for providing compound 4 for Composite 3. The report also

indicates that compound 7 was not assigned to any of the participating companies to provide for the

study by the ECA. The reason for this discrepancy and responsible party are not clear.2 Table 1. Fluoropolymers To Be Formulated Into Composites For This ECA Testing Program

Compound

Number Inventory ID #,

Accession ID #,

and/or CAS ID # Chemical Name Generic Chemical Name

1 CAS # 9002

‐ 84

‐ 0 Ethene, tetrafluoro

‐ , homopolymer PTFE

2 CAS # 25067

‐ 11

‐ 2 1

‐ Propene, 1,1,2,3,3,3

‐ hexafluoro

‐ , polymer

with tetrafluoroethene FEP

3 CAS # 26655

‐ 00

‐ 5 Propane,1,1,1,2,2,3,3

‐ heptafluoro

‐ 3

‐

[(trifluoroethenyl)oxy]

‐ , polymer with

tetrafluoroethene Modified PTFE

4 CAS # 25190

‐ 89

‐ 0 1

‐ Propene, 1,1,2,3,3,3

‐ hexafluoro

‐ , polymer

with 1,1

‐ difluoroethene and

tetrafluoroethene THV

5 DCN # 63040000026 ETFE ETFE

6 CAS # 35560

‐ 16

‐ 8 1

‐ Propene, 1,1,2,3,3,3

‐ hexafluoro

‐ , polymer

with ethene and tetrafluoroethene HTE

7 CAS # 9011

‐ 17

‐ 0 1

‐ Propene, 1,1,2,3,3,3

‐ hexafluoro

‐ , polymer

with 1,1

‐ difluoroethene Fluoroelastomer

Copolymers

8 CAS # 54675

‐ 89

‐ 7 1

‐ Propene, polymer with 1,1

‐ difluoroethene

and tetrafluoroethene Base Resistant Elastomer

9 CAS # 27029

‐ 05

‐ 6 1

‐ Propene, polymer with tetrafluoroethene Base Resistant Elastomer

10 CAS # 26425

‐ 79

‐ 6 Ethene, tetrafluoro

‐ , polymer with

trifluoro(trifluoroethoxy) ethene Perfluoro Elastomer

11 CAS # 9010

‐ 75

‐ 7 Ethene, chlorotrifluoro

‐ , polymer with 1,1

‐

difluoroethene CTFE Elastomer

12 CAS # 31784

‐ 04

‐ 0 Ethene, tetrafluoro

‐ , polymer with

trifluoro(pentafluoroethoxy)ethene Not Available

13 DCN # 6304000018A Polytetrafluoroethylene Polytetrafluoroethylene

14 DCN # 6304000018B Polytetrafluoroethylene Polytetrafluoroethylene

15 DCN # 6304000018C Fluoroelastomer Fluoroelastomer

16 DCN # 6301000018D Fluoroelastomer Fluoroelastomer

17 ACC # 137678 Low Temperature Fluoroelastomer Low Temperature

Elastomer

EPA	states	that	“the	documented	composition	of	Composite	#3	doe s	not	seem	to	comply	with	the

stipulations	of	the	ECA	test	pro tocol”,	noting	that	CAS	25190‐8 9‐0	and	CAS	9011‐17‐0	were

apparently	not	include d	in	Composite	#3.

During	the	call,	we	confirmed	that	the	term	“test	protocol”	ref ers	to	the	“Quality	Assurance	Project

Plan	for	the	ECA	Incineration	Te sting	Program	–	Phase	II	Fluoro polymers	Incineration	Testing”

(QAPP).			The	Composit e	Preparation	Report	for	Composite	#3	(fl uoroelastomers)	is	contained	in

Appendix	28	to	the	Final	Study	R eport.		Report	Table	1	and	the supporting	information	in3 Appendices	ARDL‐C	and	ARDL‐D	show	that	3	of	the	materials	added to	Composite	#3	were	not

identified	with	a	CAS	number,	a pparently	in	order	to	protect	co nfidential	business	information

(CBI).			Unlike	the	Study	Director,	the	QA	Unit	for	the	project had	access	to	confidential	identity

information	for	the	ma terials	sent	by	the	companies	to	form	the composites.		As	the	QA	Unit’s

Composite	Preparation	Report	Rev iew	for	preparation	of	the	fluo roelastomer	compos ite	at	ARDL	in

Appendix	1	to	the	Fina l	Study	Report	shows, “The	documented	com position	of	this	composite	is	as

described	in	Attachment	8	of	the QAPP	with	tabulated	components as	described	in	Attachment	7	of

the	QAPP.”		In	order	to	ensure	th at	the	Final	Study	Report	woul d	not	contain	CBI,	the	companies

claiming	CBI	on	the	identity	of their	contributions	to	a	test	s ubstance	composite	sent	non‐redacted

copies	of	the	Chain	of	Custody	Form	(used	to	transmit	samples	t o	ARDL)	to	Docket	OPPT‐2003‐

0071	at	the	EPA	OPPT	Document	Control	Office	that	included	the confidential	CAS	numbers	for	the

material(s)	pursuant	to	Section XIV.D	of	the	ECA.		Therefore,	E PA	staff	has	access	to	the	confidential

identity	information	provided	by	the	Companies	that	can	be	used to	confirm	the	QA	Unit’s	finding

that	Composite	#3	was	prepared	in	accordance	with	the	requireme nts	of	the	QAPP.

Area #2

– Deviation from QAPP

Table 2 below provides a summary of the facilities responsible for the major activities related to Phase II

incineration testing for the fluoropolymer incineration study. For each major activity, the table lists the

facilities specified in the QAPP and the actual facilities specified in the final report that performed the

task. The principle deviation in the facilities from the QAPP is the inclusion of Akron Rubber

Development Laboratory, Inc. and Shealy Environmental Services, Inc. for compositing and analysis.

Additionally, Exygen Research was purchased by MPI Research and is referenced in the final study report

as MPI Research.4 Table 2. Facilities Responsible for the Activities Related to Phase II Incineration Testing for the

Fluoropolymer Incineration Study

Activity Facility Specified in QAPP Actual Facility Specified in Final

Report

Supply of fluoropolymer

components AGC Chemicals Americas, Inc.

(Bayonne, NJ); Clariant GmbH

(Charlotte, NC); Daikin America,

Inc. (Orangeburg, NY); E.I. du

Pont de Nemours and Company

(Wilmington, DE) AGC Chemicals Americas, Inc.

(Bayonne, NJ); Clariant GmbH

(Charlotte, NC); Daikin America,

Inc. (Orangeburg, NY); E.I. du

Pont de Nemours and Company

(Wilmington, DE)

Compositing fluoropolymer

composites StereoChemical, Inc. (Newark,

DE) Composites 1, 2, and 4:

StereoChemical, Inc. (Newark,

DE)

Composite 3: Akron Rubber

Development Laboratory, Inc.

(Akron, OH)

Composite analysis (carbon and

hydrogen and percent solids) Exygen Research (State College,

PA) Akron Rubber Development

Laboratory, Inc. (Akron, OH)

Composite analysis (total

fluorine and percent solids) StereoChemical, Inc. (Newark,

DE) StereoChemical, Inc. (Newark,

DE)

Incineration testing facility

(combustion stoichiometry, TGA,

ATRS operation, and exhaust gas

monitoring) UDRI (Dayton, OH) UDRI (Dayton, OH)

Impinger samples and field

blanks analysis (PFOA and total

fluorine) Exygen Research (State College,

PA) PFOA: MPI Research (formerly

Exygen Research)

Fluoride ion: Shealy

Environmental Services, Inc.

(West Columbia, SC)5 EPA	indicates	apparent	discrepanc ies	between	the	facilities	spe cified	in	the	QAPP	and	those	who

performed	the	work	for	the following	activities:

a.	Preparation	of	fluo ropolymer	composites,

b.	Composite	analysis	fo r	carbon	and	hydrogen,

c.	Impinger	analysis	f or	fluoride	ion,	and

d.	Name	change	of	Exygen	Research	to	MPI	Research.

a.

Section	A4	of	the	EPA‐approved	Q APP	(page	11)	notes	that	Edward Gaffney	of	StereoChemical,	Inc.

(Newark,	DE)	will	serve	as	compo siting	facility	Task	Manager	fo r	those	composites	prepared	by

StereoChemical,	Inc.	and	that	J on	Kopsky	of	Akron	Rubber	Develo pment	Laboratory	(ARDL)	will

serve	as	compositing	facility	ta sk	manager	for	one	or	more	test substance	composites.		Hence,	the

same	two	facilities	specified	in the	QAPP	for	composite	prepara tion	were	used	for	composite

preparation	as	noted	in	the	Final	Study	Report.

b.,	c.,	d.

Section	C1.4	of	the	EPA‐approved QAPP	describes	the	Corrective Action	approach	used	for	this

project.		As	noted	in	QAPP	Sectio n	C1.4,	“Corrective	action	is the	process	of	identifying,

recommending,	approvin g,	and	implementing	measures	to	correct	... deficiencies	...	or	deviations

from	the	approved	QAPP.”			Therefore,	the	Corrective	Action	pro cess	was	used	during	this	project

where	necessary	to	make	revisions to	aspects	of	the	QAPP	needed to	achieve	the	data	quality

objective	for	the	project.		Corre ctive	Action	Forms	documenting required	changes	to	the	QAPP

made	in	accordance	with	Section C1.4	of	the	QAPP are	included	i n	the	Quality	Assurance	Summary

in	Appendix	1	to	the	Final	Study	Report.		Pursuant	to	Section	C 2.1	of	the	QAPP	and	Section	XIV.A	of

the	ECA,	the	companies	submitted	interim	progress	reports	every 180	days	during	the	project

containing	QA/QC	Status	Reports that	included	reporting	on	such corrective	actions.

b.

As	the	Corrective	Action	Form	da ted	December	6,	2007	(in	Append ix	1	to	the	Final	Study	Report)

shows,	MPI	Research	(formerly	c alled	Exygen	Research)	discontin ued	carbon	and	hydrogen

analysis	testing,	triggering	the need	to	identify,	recommend,	a pprove,	and	implement	a	replacement

laboratory	to	perform this	analysis.		This Corrective	Action	Fo rm	was	used	to	revise	the	QAPP	to

name	Akron	Rubber	Development	Labo ratory	at	2887	Gilchrist	Road in	Akron,	OH	as	the	laboratory

for	carbon	and	hydrogen	analysis of	test	substance	composites	f or	this	project.		Interim	Report	No.

5	(dated	December	21,	2007)	informed	EPA	of	this	facility	chang e	and	the	related corrective	action.

c.

As	the	Corrective	Action	Form	dated	August	28,	2009	(in	Appendi x	1	to	the	Final	Study	Report)

shows,	MPI	Research	(formerly	c alled	Exygen	Research)	had	diffi culty	meeting	the	sensitivity

requirements	for	analyzing	fluor ide	ion	in	impinger	samples	via ion	chromatography	(IC)	during

the	Phase	II	Fluorotelomers	project.		Consequently,	Shealy	Envi ronmental	Services (West	Columbia,

SC)	was	identified	as	a	qualifie d	laboratory	to	conduct	fluorid e	ion	analysis	via	IC	for	the	Phase	II

Fluoropolymers	project.		This	re vision	to	the	QAPP	was	document ed	in	the	Corrective	Action	Form

noted,	and	this	Corrective	Acti on	Form	was	included	in	Appendix 1	to	the	October	2009	Final	Study

Report.

d.

As	noted	by	EPA,	Exygen	Research (State	College, PA)	was	purcha sed	by	MPI	Research	and	changed

its	name	to	MPI	Research.		This name	change	was	documented	in	a Corrective	Action	Form	dated6 June	8,	2007	(included	in	Appendix 1	to	the	Final	Study	Report) .		This	Corrective	Action	Form	is

included	in	Appendix	1	t o	the	Final	Study	Report.		Interim	Repo rt	No.	3	(dated	December	29,	2006)

to	EPA	included	contemporaneous information	on	the	acquisition of	Exygen	by	MPI.		Interim	Report

No.	4	(dated	June	29,	2007)	to	EPA	noted	the	name	change	and	re sulting	corrective	action.

Area #3

– O

‐ ring a source of F?

During Composite 2 incineration testing of the previously

‐ completed fluorotelomer Phase II incineration

study, unsteady oxygen and carbon dioxide exhaust concentrations, perhaps due to exhaust gas leaks,

led to reactor system repairs. The repairs included replacing corroded stainless steel tubing and

replacing the reactor exit

‐ end silicone O

‐ ring with a higher

‐ temperature

‐ rated perfluoroelastomer O

‐

ring. This perfluoroelastomer O

‐ ring remained in service during all fluoropolymer Phase II incineration

testing. EPA would like to better understand if the observed fluoride ion concentrations in the impinger

samples may be the result of the O

‐ ring used in the reactor system as well as the combustion of the

fluoropolymer composites.

The final report concludes that the fluoride ion concentration resulting from the experimental runs are

due entirely to the combustion of the fluoropolymer composites. This conclusion was made with the

following statement on page 16 and 17 of the final report:

“Fluoride ion analytical results for the pre

‐ test steam cleanings (in contrast to pre

‐ test

thermal blanks) indicate that degradation of the perfluoroelastomer O

‐ ring on the

reactor exit is the primary source of fluoride ion in the impingers under post

‐ run steam

cleaning conditions. (These conditions include higher exit end fitting temperature and

much higher exhaust gas water concentration than during experimental runs.) Hence,

the fluoride ion results for the experimental runs correspond directly to the combustion

of the fluoropolymer composites, independent of O

‐ ring degradation during steam

cleaning.”

EPA finds a potential issue with using a perfluoroelastomer O

‐ ring as a corrective action to repair a leak

in the exhaust gas line and with concluding that its use had no effect on the results for experimental

runs. The impinger results for the thermal blanks also contained a detectable concentration of fluoride

ion ranging from 0.031 to 0.12 mg/L (approximately ten

‐ to twenty

‐ times less than the combustion

experimental run results). The contribution of fluoride ion during the thermal blank runs may also be a

result of O

‐ ring degradation. Therefore, EPA wants to know if it is possible that a portion of the fluoride

ion present during the experimental runs may also be a result of O

‐ ring degradation.

EPA	asks	about	the	potential	cont ribution	of	perfluoroelastomer O‐ring	degradation	under

experimental	run	conditions	to	fluoride	ion	results	for	experim ental	run	impinger	samples.

We	are	looking	into	this	questi on	and	plan	to	respond	to	the	Ag ency	on	this	area	at	a	later	date.7 Area #4

– CGA Concerns

Issues were encountered during testing that involved the continuous gas analyzer (CGA). During the

post

‐ run thermal blank for the third run, the CGA unexpectedly shutdown and the post

‐ run thermal

blank had to be rerun. As a result of this issue, the CGA was serviced by the manufacturer prior to the

seventh set of runs. It is noted in the final report on page 47 that the pressure drop across the CGA

decreased to 14 inches W.C. during the final six runs compared to 22 inches W.C. that was observed

during the first six runs. It was also noted that the records for the recalibration of the CGA after it was

serviced were not provided (see response to Subtask 8). It is not clear how this pressure drop may have

affected the final results or if it had any effect at all.

Additionally, during part of the ninth post

‐ run steam cleaning and all of the twelfth post

‐ run steam

cleaning, the CGA was connected to the reactor system exhaust gas. The established protocol was to

not have the CGA connected during steam cleanings to prevent condensation from occurring in the

tubing of the machine. It is not clear how this affected the final results or if it had any effect at all.

EPA	raises	questions	about	(a)	r ecalibration	of	the	continuous gas	analyzer	(CGA)	following	service

by	the	manufacturer	prior	to	beginning	Run	7	(see	page	47	of	Fi nal	Study	Report),	(b)	the	potential

impact	of	the	change	i n	pressure	drop	acro ss	the	CGA	as	a	resul t	of	such	service,	and	(c)	potential

effect	of	the	CGA	being	connected to	the	reactor	system	exhaust during	post‐run	steam	cleaning	for

part	of	Run	9	and	all	of	Run	12.

(a)	As	the	October	7,	2009	Corre ctive	Action	Form	by	Richard	St riebich	on	this	subject	(in	Appendix

1	to	the	Final	Study	Report)	shows,	the	ABB	(CGA	manufacturer) service	engineer	visited	the	UDRI

lab	on	August	3,	2009.		As	a	result	of	his	diagnosis	of	the	cau se	of	the	unexpected	shutdown	of	the

CGA	during	the	Run	3	Post‐Run	Thermal	Blank	on	July	30,	2009,	t he	ABB	service	engineer	bypassed

the	malfunctioning	CGA	flow	sens or.		This	ABB	field	service	vis it	did	not	include	conducting	or

providing	a	record	for	calibrati on.		Following	the	August	3,	20 09	service	and	prior	to	beginning	Run

7,	the	CGA	was	recalibrated	by	U DRI	on	August	3,	2009	as	descri bed	in	Richard	Striebich’s	notebook

pages	62‐63	(in	Appendix	36	to	the	Final	Study	Report).		These notebook	pages	constitute	the

records	for	this	recalibration.

(b)	We	are	still	looking	into	t he	pressure	drop	question	and	pl an	to	respond	to	the	Agency	on	this

sub‐area	at	a	la ter	date.

(c)	Richard	Striebich	prepared	a separate	October	7,	2009	Corre ctive	Action	Form	(included	in

Appendix	1	to	the	Fina l	Study	Report)	regard ing	the	connection of	the	CGA	to	the	reactor	system

exhaust	gas	during	post‐run	stea m	cleaning.		Standard	practice aimed	at	prevent ing	excess	water

entering	the	CGA.		However,	the	CGA	was	inadvertently	left	conn ected	to	the	reactor	exhaust	during

the	first	20	minutes	of	the	75	minute	water	injection	phase	of the	Run	9	post‐run	steam	cleaning

and	for	the	complete	75	minute	water	injection	phase	of	the	Run 12	post‐run	steam	cleaning.		As

this	Corrective	Action	Form	indi cates,	excess	water	entering	th e	CGA	during	these	two	situations

resulted	in	artificial	CO	spikes	due	to	the	overlap	of	the	infr ared	absorbance	spectra	for	water	and

CO.		As	the	CGA	graphical	output	in	Appendix	67	to	the	Final	St udy	Report	shows,	the	CGA	readings

for	CO,	CO 2 ,	and	oxygen	during	both	the	Run	9	and	the	Run	12	Post‐Run	Ther mal	Blanks	(following

the	corresponding	Steam	Cleanings )	returned	to	levels	comparabl e	to	the	Pre‐Run	Thermal	Blanks.8 Therefore,	there	was	no	lasting	effect	of	the	inadvertent	intro duction	of	excess	water	to	the	CGA

during	the	Run	9	and	Run	12	Steam	Cleanings.

Area #5

– Table 18 Fluoride Ion Recovery

The results in this table show that the fluoride ion recovery greatly varied from as low as 58% to as high

as 120%. The report did not offer any explanations as to the reason for the deviations in recovery.

Further, the study did not subtract any estimate of baseline fluoride ion levels due to degradation of the

O

‐ ring: the measured fluoride ion concentration and measured impinger water volume were used to

calculate the recovered fluoride ion. The presence of a baseline level of fluoride ion could potentially

account for the fluoride ion recoveries greater than 100% but would not account for the fluoride ion

recoveries less than 100%.

EPA	notes	that	the	report	did	not	explain	the	reason	for	fluori de	ion	recovery	values	in	Table	18

ranging	from	58%	to	120%.

As	Section	II.F.4.b(1)	of	the	Fi nal	Study	Report	(p.	56)	notes, “Comparison	of	experimental	run

fluoride	ion	results	to	predicted	fluoride	levels	in	the	imping ers	yield	recoveries	between	70%	and

130%	for	at	least	two	of	three	ru ns	for	each	composite.”		We	fo cused	on	closing	the	fluoride

material	balance	within	70%	to	1 30%	for	two	of	three	runs	based on	the	two	out	of	three	logic	used

in	Section	C.2.5.5	of	Appendix	C	to	the	ECA	(QAPP	Attachment	2)

.

Notwithstanding	that	logic,	all of	the	experimental	run	results for	fluoride	had	re coveries	within	the

50%	to	150%	range,	which	is	str ong	performance	considering	the small	quantities	of	fluoride	in	the

system	needed	to	assure	that	theo retical	thermal	reactor	system exhaust	HF	concentrations	were

consistent	with	uncontrolled	HF emission	levels	from	full‐scale municipal	waste	combustors	as

noted	in	Section	II.F.4.b(2)	of	the	Final	Study	Report	(p.	57). This	consistency	helped	assure	that

thermal	reactor	system	operations were	representative	of	typica l	full‐scale	municipal	waste

combustor	operating	conditions.

As	the	Discussion	of	Results	in	Se ction	II.F.4	of the	Final	Stu dy	Report	(pp.	53‐55)	demonstrates,

laboratory‐scale	testing	was	cond ucted	within	the	ranges	specif ied	in	the	EPA‐approved	QAPP	for

the	four	primary	factors	specified	in	the	QAPP	to	assure	that	l aboratory‐scale	testing	was

conducted	under	conditions	repre sentative	of	typical	full‐scale municipal	waste	combustor

operations:	(1)	temperature,	(2) gas	residence	time,	(3)	exhaus t	gas	oxygen	concentration,	and	(4)

exhaust	gas	water	concentration. Consistency	between	theoretic al	thermal	reactor	system	exhaust

HF	concentration	and	available information	on	uncontrolled	HF	e mission	levels	from	full‐scale

municipal	waste	combustors	provi ded	a	fifth	assurance	that	this laboratory‐scale	testing	was

conducted	under	conditions	repre sentative	of	full‐scale	municip al	waste	combustor	operations.

Area #6

– Other Perfluorinated Compounds

The identity of the ions associated with some peaks in the chromatograms at various points during the

experiment were not clear. What is the likelihood that there were other perfluorinated compounds

present in the samples?9 EPA	notes	that	the	identity	of	ions	associated	with	some	peaks in	the	chromatograms	were	not

clear.

We	appreciate	the	Agency	clarifyin g	during	the	call	which	chrom atograms	were	being	referred	to.

We	are	looking	into	this	questi on	and	plan	to	respond	to	the	Ag ency	on	this	area	at	a	later	date	after

we	are	able	to	get	assistance	from	resources	familiar	with	the LC/MS/MS	method.

Area #7

– Exhaust Gas Data

Data were not found to support the estimate of an exhaust gas concentration of water of ~15 vol%

(calculated range of 8

‐ 20%) for all Phase II experimental runs. The only support for this statement is the

sample stoichiometric calculations provided in Appendix 10.

EPA	indicates	that	the	only	support	for	exhaust	gas	concentrati on	of	water	in	the	Final	Study	Report

is	in	the	stoichiometric	calculations	in	Appendix	10.

Section	A7.1	of	the	approved	QAPP	(page	14)	includes	the	follow ing	measurement	performance

criterion:

 Operation	of	the	thermal	reactor system	to	provide	a	water	conc entration	in	the

exhaust	gas	of	approximately	15%	and	the calculated [emphasis	added]	water

concentration	in	the	exhaust	gas	within	the	range	of	8%	to	20%.

Accordingly,	the	main	method	for	demonstrating	exhaust	gas	wate r	concentration	was	indeed	via

the	stoichiometric	calculations	i n	Appendix	10.			As	Section	F. 4.a(3)	of	the	Final Study	Report	(page

55)	also	states,	MSD	(mass	select ive	detector)	monitoring	data in	Appendix	45	indicate

approximate	water	levels	between 11.7%	and	14.4%	during	the	the rmal	blanks	and	experimental

runs.

Area #8

– Calibration and Material Certs

During both Phase I and Phase II testing, a Florite 990 M2C2 universal flow controller was used to

control the flow rates of synthetic air, nitrogen, and the designated calibration gas through their

respective mass flow controllers. While calibration records and certificates are provided for the

individual mass flow controllers, these data are not provided for the universal flow controller itself.

Additionally, during Phase II testing, the CGA aborted itself during the post run thermal blank after the

third experimental run. As a result, the equipment was serviced by a technician from the equipment

manufacturer and recalibrated. A calibration certificate and records of the calibration were not

provided for the recalibration of the CGA after the service was performed.

In	addition	to	apparently	repeatin g	the	first	part	of	Area	#4, EPA	asks	about	calibration	records	for

the	Florite	990	M2C2	uni versal	flow	controller.10 The	Florite	990	M2C2	universal	f low	controller	(UFC)	is	an	inpu t‐output	device	that	provides	a

digital	interface	with	the	Brook s	mass	flow	controllers.		As	su ch,	we	are	not	aware of	any	calibration

record	or	certificate	that	accomp anied	the	Florite	990	M2C2.

Detailed	calibration	information	for	the	actual	flow	metering	d evices	(the	Brooks	mass	flow

controllers)	is	presented	i n	Appendices	11	and	40.

During	the	Phase	II	Fluoropolyme rs	project,	UDRI	checked	the	ov erall	flow	measurement	system

(Florite	UFC	plus	Brooks	MFCs)	to confirm	accurate	gas	flow	mon itoring;	this	overall	flow	check	is

presented	in	Appendix	43	to	the	Final	Study	Report	along	with	t he	Certificate	of	Assessment	for	the

NIST‐traceable	Agile nt	ADM‐2000	used	to	check	these	flows.