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COHKOnBALTB OP VIRGINIAD.partm.D~ of Air Pollu~ioD COD~rol
INTRA-AGBNCY JlBH()JUUmUX
'1'0: File
PROX: R. o. Goetz
SUBJECT: DUPONT, WAYNESBORO, REGISTRATION '20517
DATE: October 12, 1989
RE: STACK TEST 10-6-89 NEW DMF SCRUBBERS ON ORLON FIBER DRYERS
A witnessed stack test was performed 10-6-89 on one of two ('2scrubber, near river) new large scrubbers for DMF (VOC) scrubbingefficiency, inlet and outlet concentrations and pounds per houremission rates. The scrubber tested was fUlly loaded (one-halfscrubbing capacity) by full production on one-half (3) of the sixorIon fiber dryers.
Opacity was always zero (ot) except for a short moisture plume- VEE's attached.
See the attached stack test monitoring sheet and proposed testprotocol by ETS for more details.
"Preliminary" results indicate (average of three one hourtest runs):96.6t scrubbing efficiencyInlet DMF: 332 ppm, 175.5 lb/hrOutlet DMF: 11.6 ppm, 5.9 lb/hrDMF concentration in scrubber water reservoir: 2.6tPlant hopes to increase this to 9 or lot for more efficientrecovery.Inlet feed water: 4000 lbs/hr -- 8 gal/min.Ran about six days before test day.
PBBSOIQfBL PRESBNT
duPontRon Shifflett - EnvironmentalPaul Dana - Orlon Process Enqineer - Scrubber "father"Merv Meckley - Wilminqton, Del. - "Scrubber designer"Jim Harris - Orlon manufacturinq supervisorEd Monqan - EnvironmentalGeorqe Aylor - Retired duPont - construction coordinatorDavid Hopkins - Fiber Dryers
Ed HandelTony UnderwoodLori Graves
~Ray GoetzSam Barnard (VEE)
RaYmond O. GoetzEnqineer, Region II
ROG/bh
Attachments
cc: -Division of Technical EvaluationS. K. Barnard
--.
'.-lJ. Nor-tOlilu\ I'll Bm-I' (NCS :1. C lo'AI.:-l'olt2. J\SSlrro1ED r~~l\JRE -C-ON-T-£N-'r---'-'--3. INlJTCJ\'1'IW NOZZLE: ~nZE -- ----------
C:. ~J\Ml·l.lN(; l~HOc:I:;DURE ---.----------1. r.Jo:J\K CHECK DONE: 1i~~FO~ ~ AJo~TER ~
~) • "1'1'( )'1' . '1'111\1,:: 'loy 1'1:; ~ ~~_ ~...l. '1'Y' '\::',1' ----.~. NOZ1.L":~;I Zl-: U~;~: . - .~.4 , 'r114£ A'r EACH P'.\'.: I "=>5. 'l'O'1'AL TIME OF TEST~:-+-\-M=~-Le..,-~~-'---........J-~--6. 'l'ES'1' INTERRuPTED: NO -'. n:S(EXPLA.liL~
b, SAMPLE CLEAN-UP -------.----1. FILTER HANDLED CAREFULLY: ·YES ,n. ,A. . NO2. Jo''[L'1'ER HOLDER WASHED 00'1': YES. n. +: 110 ----3. PROBE WASHED OUT: YES --- BO4: CYCLONE 'WASHED OUT : YES A. A NO ----5, WASIIINOS SAVED: YES NO
MA'rEIUAL ma.:u: PI . 7,~ ----,------------]v;.- A1}IH'l'IONAr. COMMEN'l'S: . . . • .
I i) - a::.-::- '!- , ~ . ...,..r .... .. u..;;:..~2 II ":J..6~/~:J I ---~ -0-'5 v Ie-:-I, ~3 1~.1.17-11('f7 -~_.u~V,;-
. . 'i: t( ;.., f 7 - I g 17 - ~~ _." ~ ~""- tf I ~~ eJ.M., t, 'ti::d-~...,a. ...~~~~'ti..;,
COMPLIANCE TEST REPORT
FOR
E. I. DUPONT DMF SCRUBBER NO.2
LOCATED IN
WAYNESBORO, VA
OCTOBER, 1989
ETS, INC.
A subsidiary of ETS International, Inc.SUITE C-103
3140 CHAPARRAL DRIVE
ROANOKE, VA 24018
,OCT 1 2.1989
11 J. ()r-/1
--
Pollution Control ConsultantsSpecializing In
Toxic Emission Measurement and ControlETS CONTRACT NO. 89-210-T
RBPORT CBRTIFICATION
I have reviewed all testing details and results in this
report and hereby certify that the test report is authentic and
accurate.
DATE: ~Mw fdr:t~
SIGNATURB:~ ~Edward D. Handel. PhDSenior ChemistETS. Inc.
I have reviewed all testing details and results in this
report and hereby certify that the test report is authentic and
accurate.
DATE: CJ::,fv1,.,.. I V/ I C-;_~_"..:...tt_---,.,
SIGNATURE:~£-1/#~~;-WrightManager/Technical ServicesETS. Inc.
I have reviewed all testing details and results in this
report and hereby certify that the test report is authentic and
accurate.
~..~~.~~ /' JOSEPH ••••• 0 ~*' : .. \ 1},• r. • I:
"G! SZAL~Y ! Iti• • llJi,'tJ '•• ~ 15225 .:" 411\.0 '. ~ ().' l
~A ".~'STE~~'···. ,~'l.''':6. •••••••• '=': ....v& ~.'
IONA\..~·..•••.......,..........'"
P.B.: E-Ol5225
S TA TE OF: _--=-O.:.:hc..::i..=:o _
TABLE OF CONTENTS
1.0 INTRODUCTION ," .. .. .. .. .. .. .. .. .. .. .. .. .. .. 1
2.0 TEST PROCEDURES.................................... 32.1 DMF GAS CONCENTRATION......................... 32.2 MOISTURE CONTENT.............................. 42.3 TOTAL GAS FLOWRATE............................ 42.4 WASTEWATER ANALySIS........................... 42 .. 5 PROC BSS DATA.. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. .. 5
3.0 SAMPLING AND TEST METHODOLOGy...................... 53.1 OMF ANALySIS.................................................................... 6
4.0 RBSULTS ......•..............•...................... 6
LIST OF TABLES
TABLE 1 - RESULTS OF EFFICIENCY TESTING ONSCRUBBER NO.. 2.............................................................. 8
LIST OF FIGURES
FIGURE 1 - SCRUBBER SYSTBM ........................................................... 9
FIGURE 2 - SCRUBBER SCHEMETIC ...................................................... 10
FIGURE 3 - SAMPLING TRA IN .............................................................. 11
FIGURE 4 - TRAVERSE POINT LOCATIONS FOR INLET DUCT ...... 12
LIST OF APPENDICES
APPENDIX A - COMPLIANCE -TEST LOG........................ 13
APPENDIX B - STACK VELOCITY DATA FIELD SHEETSAND CALIBRATION DATA FOR SAMPLING PUMPS 14
APPENDIX C - ANALYTICAL METHODS 23
APPENDIX D - ANALYTICAL DATA............................ 28
APPENDIX E - PLANT OPERATIONAL DATA..................... 55
1.0 INTRODUCTION
A compliance test program was ~erfor.ed on the new wet
scrubber system installed on the orl~ process at the duPont
Waynesboro Plant. The testing program was designed to determine
the level of abatement of N.N-Dimethylformamide (DMF) emissions.
Compliance testing was performed on only one scrubber (desig-
nated Scrubber No.2) at this time. Scrubber No. I will .be
tested on a subsequent date. Testing was performed by L. Graves,
T. Underwood and T. Handel of ETS, Inc. on Friday, October 6,
1989. The testing was coordinated with P. Dana and R. Schifflett
of duPont. All operations data was collected by duPont personnel
and has been included in this report as Appendix E. The test
program was witnessed by R. Goetz of the Roanoke office of the
State Air Pollution Control Board.
The test program consisted of three rePlicat, series of
measurements. All testing was conducted while the\Jrlon process
was operating normally. Plant operations data were collected for
each of the testing periods. This information is included as
Appendix E. Each series of tests consists of the following
measurements:
1) DMF gas concentration at the inlet duct of the dual
scrubber system.
2) DMF gas concentration at the outlet of Scrubber No.2.
3) Total gas volumetric flowrate at the inlet duct of the
scrubber system.
-1-
4) Moisture content of the inlet duct of the scrubber
system.
5) Moisture content of the outlet duct of the scrubber
6)
~7)
system.
DMF concentration in the scrubber system wastewater
effluent.
OrIon process operational data.
DMF
All inlet/outlet testing was performed simultaneously in
order to evaluate rea) time scrubber efficiency.
Figure I illustrates the overall gas flow details for the
system. The scrubber system is designed with two
units, each designed to handle up to 75,000 actual
cubic eet per minute (acfm) of exhaust gases. With both
in operation, the combined exhaust gases from the six
rs. the Pidler exhaust and the waste exhaust unit can
be treated simultaneously. Due to a lack of demand for OrIon
product. only one scrubber was conditioned for testing at this
time. Scrubber No. I was isolated from the system and was not
involved in the current series of tests.
Figure 2 shows the details of the scrubber construction.
Each unit is equipped with an 800 HP blower to force the inlet
gas through each scrubber. In the current test program, only the
blower to scrubber No. 2 was operated.
-2-
2.0 TEST PROCEDURES
The rectangular inlet duct is 96 inches wide and 80 inches
tall, with an effective diameter of 87 inches (7.3 feet). Three
inlet sampling ports were located 56 feet downstream from the
particulate screen and 14 feet upstream from the beginning of the
right angle bend of the duct. Each port was three inches in
diameter. Outlet sampling ports are located at the top of each
scrubber, as shown in Figure 2. The diameter of the scrubber
outlet stack is 8 feet.
Bach sampling run was conducte for a period of 60 minutes
at a nominal sampling rate of 1.5 per minute. Both inlet
and outlet sampling was performed using the center of the
respective ducts as the point of sample withdrawal.
-3-
The impinger solutions and the sorbent tube samples were
analyzed using GC/FID in accordance with the general conditions
outlined in NI08H Method 2004. The impinger solution volumes
were measured and recorded. Impinger 2 and 3 contents were
combined and analyzed. Impinger I was analyzed separately. The
probe and connecting lines were rinsed with deionized water. The
probe wash volume was measured and the solution was analyzed for
DMF.
2.2 Moisture Content
Moisture content of the inlet and outlet gas streams was
determined by measuring the volume of water gain in the three
impingers in the sampling train.
2.3 Total Gas Flowrate
volumetric flowrate of the inlet gases was
velocity traverses in accordance with BPA Methods
(40 CFR. Part 60. Appendix A). Four traverse points
were used in each of the three inlet ports. giving a total of 12
traverse points (see Figure 4). The traverses were conducted
before and after each of the DMF sampling runs. The traverses
were performed using a Type "8" pitot tube. a type "K" thermo
couple. and a digital manometer. Field data sheets for the stack
velocity measurements are contained in Appendix B.
2.4 Wastewater Analysis
A sample of the scrubber wastewater was withdrawn during
each run. These samples were analyzed for DMF concentration by
the ETS Mobile Laboratory utilizing the same procedures used to
analyze the impinger solutions. The Analytical Method is
contained in Appendix C and the results of the analytical
determination of DMF are contained in Appendix D.
2.5 Process Data
Data collected by dUPon~Plant personnel
operation of the OrIon process~and associated
included in this report as Appendix E.
3.0 SAMPLING AND TEST METHODOLOGY
regarding the
scrubber system is
All sampling was conducted using sampling pumps calibrated
onsite before and after each run. Each pump was calibrated with
the sampling train in place ting an inverted bubble flowmeter.
Calibration data is containe in Appendix B. Each sampling train
was the leak checked precedi sampling interval by plugging the
tip of the sampling probe and observing
bubbling in each of the impingers. The
the c~ete cessation
rotameter was also
of
observed to insure that no leaks were present in the sampling
train.
Sampling was coordinated using radio communication to ensure
that inlet and outlet sampling was conducted simultaneously.
-5-
3.1 DMF Analysis
DMF analysis was performed onsite in the ETS Mobile Labora-
tory located at the foot of the DMF scrubbers. Analysis was
begun immediately following each sampling period. The analysis
was performed on a Shimadzu GC-14A gas chromatograph equipped
with a flame ionization detector (FID). The analysis was
performed using the following conditions:
Injection: 0.5 uL direct on-column
Injector Temperature: 250°C
Detector: FID
Detector Temperature: 220°C
Column: 10-meter, 0.53mm i.d. FSOT (Alltech SuperoxII)
Carrier: Nitrogen (3.0 mL/min)
Column Temperature: 100°C Isothermal
Samples were analyzed together with standards, spikes and
duplicates.
4.0 RESULTS
Test r~was aborted during the test due to a power
failure. The compliance data consists of three consecutive
tests (runs 2, and 4) performed on Friday October 6, 1989. All
outlet data contained in this report is for Scrubber No.2. The
test log for the compliance testing is contained in Appendix A of
this report. Duct flow measurements ranged between 61,000 and
-6-
68,000 acfm during the testing. The results of the DMF Compli-
ance Tests for the duPont DMF Scrubber No. 2 are contained
in Table 1.
ency
Bach of the th~ compliance tests demonstrated an effie i
of greater than 9~ercent abatement of DMF emissions.
The scrubber was operated at full capacity during each of the
tests. The specific plant operations data were provided by
duPont personnel and are contained in Appendix B of this report.
The inlet concentrations of DMF ranged between 286 and 397 ppmdv
during the compliance testing. The outlet concentrations ranged
from 17.1 to 8.9 ppmdv. efficiency
measured for the three tests was
The concentration of DMF in the wastewater in the bottom of
the stack remained relatively constant at 2.5~ throughout the
testing.
-7-
Table 1. Results of Efficiency Testing on Scrubber No.2.
Run 2 Run 3 Run 4
Inlet Temperature (0 F) : 156.8 153.4 153.3
Inlet Pressure (Static) (in. H20) : -0.999 -0.972 -0.980
Duct Velocity (ft/s): 21.5 20.2 19.0
Duct Flowrate (acfm) : 68760 64790 60950
(scfm): 56080 53130 49820
(dscfm): 51090 44460 43160
Inlet Moisture (%):
Outlet Moisture (%):
Inlet DMF Concentration (ppmdV):
Outlet DMF Concentration (ppmdV):
Inlet Emission Rate (lbs/hr):
Outlet Emission Rate (lbs/hr):
Scrubber No.2 Bfficiency (%):
Scrubber No. 2 Wastewater Analysis:
Concentration ('{w/v» before run:
Concentration {%(w/v» after run:
-8-
8.9
10.4
397
8.9
230.9
3.0
98.8
2.19
2.59
16.3
10.4
286
17.1
144.7
8.6
94.0
2.59
2.55
13.4
8.9
312
12.6
153.2
6.2
96.0
2.55
2.55
Six OrIon f1 ber dryersT\oIo exhaust fens each
1 P1dlerexhaustunit
1wasteexheustunit
Outlet Sample I.oc8tions
F1gure 1- Scrubber System
T56'
14'
1.
T'v/o Dt1FScrubberSystems
75000cfmeach unit.
1150000 cfm totall1tl. no",
Particulate SCreen
Inlet duct96" ",ide x 80" tall
Inlet sampU n9 Location
/
-9-
IIi 'I
Outlet SamplePort
fresh WaterInlet120pm
Reel rculstionWeter3500gpm
Weste'vl8terto Recovery
60pm
11I1I1I1I1111I1111I11I1111I11I111111I1IIIII111111111II1111
1
1
1
111'111
AcceS3 Platform
12 Bubble Cap TraY$
Packed Bed
~(---- Ga~ Inlet
OCT 12 1989
Figure 2 - Scrubber Schemetlc
-10-
v
~dget:i::,nlceboth.30 mh distmed water 1neech1mpi noer. Water gal ned in 1mpi nger~measured to determine moisturecontent of stack gas.
L~I:bre~PersonalSampll ng Pump
I
n
Gss flow
Stack
Teflon tubino.
"Stainless steel probe.
Sihca-GeJ Sorbent Tube150 mo front half to catch
~ any OMf throuoh 1mplnoer\ train. Beck-helfsilic8 oel\~~~t conte) n<10% of totali'i \ to ...ure no break-through.
~R ~~ CJ", D'J, 'tJ]I- ...
Figure 3 - Sampllng Train
-11-
K 96" )l
I + + + + FI/ 40"
1// 66.7"
SAMPlE-, + + + + SO"PORTS t
+ + + +I1
r12"--"1- -->4:136" .. -
~. 60" ------.o'l~
~ 84" ------....;t~End Vie'yl - gas flo'vlinto paper.
Flgure 4 - Traverse Polnt Locat1ons for Inlet Duct
-12-
APPENDIX A
Co.pliaDce Test Log
Run 1 Aborted due to power failure during test.
RUD 2
Run 3
Run 4
Start Time:
Bnd Time:
Start Time:
Bnd Time:
Start Time:
Bnd Time:
11:26
12:26
13:37
14:47
17:14
18:14
13
APPBNDIX B
STACK VBLOCITY DATA FIBLD SHEETS
AND CALIBRATION DATA FOR
SAMPLING PUMPS
14
FIELD DATA SHEET
4t'i\-'',- q75
Ib "3
({ l..
RUN NUMBER I L I'l (-<. rSTART TIME--'0---.;'3~__
END TIME
I t II
J I I100 /'J- ~1
L./ !t I./.b Ii .at, i
\ I I/' I ,I>=)--! ''J,y
! II II '1 I
I j I ,I~,i I
I I? i I?· I II21 I. >3-i £:{ !
i
,J I'. I~I_1_1_(~I5....,:,'__1 --I.l.loo-k LJI (J (! . I( '{ i f'j~ !
Ie L I
I L..P STACK 11 T STACKPOI NT I In. W.C. [I.;-g. f
I Time f6pU
, POST-TEST
Traverse Data
PRE- TESTI i I, II ;ll'i":e I I! 107.75 II II
~p STACK I T STACK\ POINTI In. w.e.
ID~g. f
IL[l .0'1.1 fJ-I
I). I qj
·o~II
J I fJ-. ~';-J- I
~\u'-,~ L{~I
?LI,ol}l I
/ ~o~I
q1! OS () 5)....
} .os'S Rtf
3 .fJ51 ?If~ .0,)- F3
l!-l I . Oyq 1/III,
j. I Viq ~II,
:> I .0 </0 Ii!
L{j .0,1 10!
• .>-ti' ?).t
Notes
II------!I II I
NET VOLUME iRATE - lprr, ICAlIB~'ATlmJ DATA
--~---~--- II Ii -,!II
NET Tlt1E
FIELD D""TA SHEET
r' t-(. ] eel ])vpDIl/r ~ - 2/C'
~ ~x~ ticn lJIfYt/c:}t>C!I:';'d 1/.:.)
[J':Jt.~ 10- h- :6'
RUN NUt-1DER
START TIME
END TIME
Traverse Data
POST-TEST
A. P '='T.'r·v IL;;;. 'J H~r·. 1
In. w.e.
Time
POINT
I!I
~I--~~'-----i------;,II
I I
i,;tee=>---'; "i I
l I~p ST~CK T 3TAU! PCq NT I Ir, \t.I r n ~i-' 1__" '_'_'._-_.--+-__!J...;~I~;.,.'_'_-!I1 j
i,
I I! ;H:-:e II I
~ I
I;--_.-.........-
Notes
--I biT JEty),
CALI Bl:.'ATION O;;TA! T! NHVOLUME ! RATE -lprr., ,
I!I NEi Tlt1E
,. 1 ?i::::!-Te~t
I
FIELD DAT A ~~HEET
RUN NUr'iEER Url(-(1-
":;.t
START TIME--------EflJDTIME 1.}J-(,
Traverse Data
, \O~I ~-'{
.lOL.{I;;
, iif,11'7
f(• r>-~
I,..;
().:) 17'(,I
.lc3 1;;-1
. II q I;-l..t
.Po (~~
vib 145
.o3l I L{ b
.t/'1L({'-If
()bo {l.(C(
3 'I' I [/C{ -il (67' il( ./1l( I tbL II I ICY III(J l, ,ffJ- I /
Notes
I )- .'J •
I (.1 !r 1>5' If,;J I
c.. l i I '1 . II I$') I,
) I I I~A~---l-I----:..'..:...I'-1}",,3-l--f~'()V;;.---o
J I IJ- It.>.-
POST-TEST
I ). I .• jDOI, I r t1tfI- I
I Time I 10 (L..P STACK T STACK 1
POINT I In.W.e. Deg. f Ii
ttl I I)~ I IG J II I
IIr--------1-----!
157
T 3TAC\(D;;I~. F
CAlIe::"ATION DATA
L {~!_'.-;../1L(~l_'1/.....:-9---11.;>.. ! I I
I .0 "It.{ I It{ i I__..:-3+!_"t!Li /-;0 I
4; .0 ( ~! /'1, I
IiI /' p' '='T '.... ,; II ~ .J H'.r., I! F'Oi NT I Ir ~M C II I d. ,... !
PP£-H'3T1 II T. ,....'" ii It • fit ,r; I " - ,, I .r I
FIt:LD D~TA SHEET
_. Pr(l] ~c t ~JeOA/r ~~- Z//c..J
~ 0Cetic'n tt/,tY've·Str.)j~U) V,-[Iljte to-fa -?2
RUN Nur'1BER_11-_~__--:t::Q:.-~_'~f:rSTAPT TIME 11:2. tv ctl,h,(..(/r/l-c. ...~
END TIME /).')..l.e.
Traverse Data
T ~3TACK
Dey. fh. P ST"'<"-K I~ 1'1·.. ··1
In. w.e. !I
POINT
POST-TEST
I Time
i---I~----...---_
;---1----.;------;i I
t---~---·-1--·----'
I I!
T STACk.D~ll F
I
! i iI I
I,---+.---,!
IT. ,_." I
~ f' 'f .-~ J I
1-'--1 II I r. p t;.'Y':~'" II __ ,._ .....11 M'.. r··. I! 1-".' "j I I I L I r .r. If.' ,I I'" I, ••• I
I I
! I----,..------!, III~I Ii , __+-~l
,----;----I 'I ~
i' I
CALlB~I~TION DATAI ,
t:ET TI ~'lE ! UET'!OLU~'lE 1 RATE - 1pm
Notes
J.~
.9 ' If) ,
/9. ~""! Sl7L.)~.-:,
,I
; 1:'., .. - ri'~t: ..
II ",'" CO-I ,,,,- t"I ~ ~ .... ,' ..... '"-' l. /.S
FIElD DATA SHEET
Pro.i ec t _O~(A,~Ot::.:.:I.,\~}- -
!..ccetion -
[late 10 -b -Z'1
RUN NUr iBER :1 )Il!-t /-.i345STAPT TIME--.;...---
END TIME Il.{vr
Traverse Data
Notes
POST -TEST
, .'7rt-tt;v '.
-- q~~
., I r { () () , !JJ !
}! \11'[ I I{;0L( I 'I()- l-,G-.l ---;
t !
).,I
I i II
Time "D) IA. P ST"f'K i T STACK I
l~ 1'1 ... ··1 IPOINT Dey. f IIn.W.C. i i
Wi ! I
.Id J /§1 !!
I .j
1-----"J-::..-+-I_\;..,;".;ll_O_1 150.....-'~Lj"3 I ,I'; I tr' II I I
P~£-TEST,II
l~~t,I T· II 11me I•1 II J /' F -=-T'r'¥ T STACKI I~ ;)",-"! PO!lH I In. V·! ,C. D~g, fI I, Ii k t ! .101 I~~Ii )- I (J £.( b-~III
I fi'! J , II~I
IiI
, (}l ( Sl)!~
I u.~~\ 0/ \ IO~ I§l
d- .(O'~ l ~)
): .rl q (t;c{. i
~I
l~t/! ,ll 0
e.l I.o~ ~ ltf.f
,I!
)..:.o~g ILl'I
I
1 .C) ~ l.l /ql---
l.\ . (41c (), 0 I II,
() ,'3\f? l<"f,7f
CAlIB~'ATIONDATAI ! !! NET TIME I NET VOLUME I RATE· 1pmI
I ! I
! I I .1;0 f 1.)0I ;:"'" -!'';;$t J{) /)0 I JC1lr I !t'(l::,!. i~~t )-C(I;q/~ I .~~O J. f. 5" Ij ,
AVEPAGE I l ('"0,i
I
RUN Nur-iSEP_-I1_~_· _~O~LI::;..nG-rSTART TIME--L:.13:=::·~i~&'~_- (.I)n~~/~'"L
END Tlt'lE JiY ¥'
FIELD DATA SHEET
F'i"O; H l 1»po~ ~-"2,/0
Leeati en t,;1'6Vta~ J/c_7
[l;jt.e 10·-1:,- «9
Traverse Data
PRE-TE~T1I ....! ;HneIJI p., ._! ') r"lI
.!I
r
/' F' -:.~. ,..", I~ JIr1I~~, I
!rl. V-!.C. IT STACKD~I~. F
POST-TEST
Time II
L.P STACK I T STACK II I
POINT I In.W.C. I D~g. f Ii
i 1I
I i
I i ,I
I I if ! I
i -1 !
II
I II
I , ! I
II
!I I
i i,,
I ,I I iI
i I
I iI I
III
I I III I
I I II I
I
CAlIB;'ATION DATA
NETTlt'lE NEi VOLUME RATE - lpm,I
: PI'''~ :~~t -:ltJ.~ svO.-.l.-- ),'1'1I i,
;.;.r~:. ~ - -;~$t ,).,O.s- aJO~ /'IyI !L.
T ~\"EPAGE /. Lj4l'I
Notes
I~ CHGc< :::. ex-C(?t.L~e-)O r J'(MJ'f' .. (7f'- '/.2 ;C
I!II
FIELD DATA 9-1~~1
RL~r.: NUf"lOEP L/ Lr, (I f-STAPT TIME__'l.o..r-'__tf__EN[I TIME ' q(L(
;",oce~ion ---:-------.~'.
Traverse Data
T STACKr'i.' ' i In, W.e. DeQ, FI i
Itl .(U( ! Ib lI .
POST-TEST
I h. P c'T "f'V1 _ -ltlT L.:i. .j':L r·, I
II Bl O'(f ira 6I ..l-..oo~_~ _
I )-! .. (0 7 (,3
ILlC( I
T 3TACVD~I~ ~. ~ ,
I: )~I
II ,I/OD I
I /' P ~·T.'~·" I
r tL,_{~j---"'--1"-!_1.7_"'_O_-i~ I I
J. \ I~D
II __ ._! 1-'1)1 r',!I
iI T1 rj~eI
,OJ.l- !
I II I I I Ie Ii U I ; Ie,;. I -;7 ~
___...3-t----'O~_]_L J if f I~ .O§5! I'-I:? I
CA1I8~'ATlON DATA
,;:,","U'AGE I ~. ) ()1--------;1L --------
FIELD DATA SHEET=#=-
F';-')jecl ])vt'OAlT'"' 8"9- 2..10 RUN NUt-mER tj ()cliUr-
~oceUon l.JA...ove5.60<:d t/:;~ START TIME J 7/ YCJi3te /O-t;.-- Y2 END TIt'1E / t/ 'i
Traverse Data
PPE- TE'3TI I II THi'le I II I 1
i STACKD~l~, F
POST-TEST
Time
lAP STACK I T STACY. II !
POINT !n,W.C, j l)~q, F i
! II
!
•I i! I ;
----~------+------;I
----+-----'1iI -
,I Ii l:~'':'- T.;'$t I
I I
CA1I8\;'Ai!ON DATA
t;n Tlt'IE tlEi VOLUME ! RATE - lpm
; I
/9,J~~ 5W~ I 1..s~
Notes
I~ ,~---&GIrl../"~hi r- rf:/"1;o .... {,s- - 70:L'
II'---__-J
APPENDIX C
ANALYTICAL METHODS
23
____-d--..-----·- ----.. __ .- -'-_ _._ .._.
FOIOOLA: (1) ~(l)N(043)2; C4H#J(2) O=OW(CHJ) 2; C3H7NO
".W.: (1) 87.12; (2) 13.10
( 1) DIMETHVLACETAMIDE and(2) DIMETHVLFORMAMIDE
tETHOD: 2004ISSUED: 5115/85
OSHA: 10 ppm (skin) [(1) and (2)] PROPERTIES: Table 1NI0SH: no standardACGIH: 10 ppm (skin) [(1) and (2)]
(1 ppm If 3.56 mg/m3 (l NTP (1)]; [1 ppm .. 2.99 mg/m3 (l NTP (2)]
SYNONYP'S: (1): !!,!!~imethylacetamide;CAS "27-19-5.(2): !!.!!~imethylfonnamide; 0f1F; CAS 168-12-2.
SAMPLING ..eASUREMENT
SAMPLER: SOLID SORBENT TUBE(silica gel, 150 mg/15 mg)
FLOW RATE: 0.01 to 1 L/min
VOL-MIN: 15 L (l 30 mg/m3
-IWC: 80 L
SHIPMENT: routine
!TE()INlQUE: GAS ()IRQf1ATOGRAPHY. F10
!AHALYTE: dimethylacetamide or dimethylfonnamide,lDESORPTION: 1 mL methanol; 1 hI' in ultrasonic
bath
!INJECTION VOLUME: 5 pL
!TEMPERATURE-IfIJECTION: 240 °CSAMPLE STABILITY: stable ~ 5 days (l 25°C [1] -efTECTOR: 320°C
-COLlm: 140 °CFIELD BLANKS: 10' (~2) of samples
RANGE STUDIED: (1): 18 to 105 mg/m3 [1];(2): 11 to 61 mg/m3 [1]
(45-L samples)
BlAS: not krom (1]
OVERALL PRECISION (sr): (1): 0.067 (1];(2): 0.056 (1]
!CARRIER GASES: N2• 50 mL/min!!COLUMN: 1.5 m It 6 nm 00 glass; 10' UCON
50~B-5100, 2\ K~ on 1001120 mesh. l Chraoosorb WHP
!CALIBRATION: analyte in methanol!!RANGE: 0.5 to 4 mg per sample (1.2]!lESTIMTEO LOO: 0.05 mg per s~le (2]
!PRECISION (sr): (1): 0.032 [1];! (2): 0.037[1]
APPLICABILITY: The ..arking range is 10 to 80 mg/m3 of either analyte for a 50-L air satf1)le.The lowr limit is determined by the desorption efficiency which ""st be detennined over therange used. Silica gel has a high affinity for water; high relative hlll'lidity will adverselyaffect the efficiency of analyte adsorption.INTERFERENCES: None identified. Separation conditions (colum. terperature. etc.) !My bechanged to cirC\IIIVent problems. Alternate colums include: 60/80 mesh Chraoosorb P coated..ith 201. UCOH L8 550X and 2\ K~; 100/120 mesh Chranosorb \ftP "lith 10\ carbowax 20P1 and 2\ KG4;100/120 mesh Chl"Q1l)S()rb .....ith 10\ SP-2250j and 5\ FFAP.OTHER M£THODS: This combines and replaces ~thods 5254 and 5255 [2].
5/15185 2004-1
(1) DIf1ETHYlACETMIDE and (2) DIMETHYlFORtWlIDE METI«)(): 2004
IREAGENTS:1. Methanol, reagent grade. '*'2. Analyte: dimethylacetamide ,
reagent grade, or dimethylformamide,reagent grade.'*'
3. Acetone, reagent grade. '*'4. Desorption efficlency (DE) stock
solution, 0.05 mg/mL Preparesolutions of dimethylacetamide ordimethylfonnamide fresh daily inacetone.
S. Hydrogen, prepurified.6. Air, filtered, compressed.7. Nitrogen, purified.
*See SPECIAL PRECAUT IONS.
EQUIPMENT:,. Sampler: glass tube, 7 em long, 6 mm 00, 4 mm 10,
flame-sealed, with plastic caps, containing twosect ions of 20/40 mesh si Hca gel (front = 150 mg;back = 75 mg) separated by a 2-mn urethane foamplug. A silylated glass wool plug precedes thefront section and a 3-mm urethane foam plug followsthe back sect ion. The pressure drop across the tubemust be less than 3.4 kPa (2.5 om Hg) at an airflowof 1 l/min. Tubes are commercially available.
2. Personal sampling pump, 0.01 to 1 l/min, withflexible connecting tubing.
3. Gas chromatograph, FlO, integrator, and column(page 2004-1).
4. Vials, 2~l, PTFE-lined crimp cap, or automaticsampler vials.
S. Microliter syringes, 10-~l and other convenientsizes for making standards.
6. Pipets, 1.0 ml, delivery.7. Volumetric flasks, 10-mt.8. Ultrasonic bath.
SPECIAL PRECAUTIONS: Acetone and methanol are flammable and a dangerous fire and explosionrisk. They are moderately toxic by ingestion and inhalation.
Dimethylacetamide and dimethylformamioe are strong irritants to skin and tissue and moderatefl re ri sks.
SAAPLING:1. calibrate each personal sampling pump with a representative sampler in line.2. Break the ends of the sampler immediately before sampling. Attach sampler to personal
sampling pump with flexible tubing.3. Sample at an accurately known flow rate between 0.01 and l/min for a total sample size of
15 to 80 L.4. cap the samplers. Pack securely for shipment.
SMPlE PREPARATION:5. Place the front and back sorbent sections of the sampler tube in separate vials. Discard
the glass wool and foam plugs.6. Add 1.0 ml methanol to each vial. Attach crimp cap to each vial.7. Agitate for 60 min in an ultrasonic bath.
CALIBRATION AND QUALITY CONTROL:e. calibrate daily with at least five working standards over the ranges 0.05 to 4 mg
dimethylacetamide or dimethylfonnamide per sample.a. Add known amounts of analyte (neat or diluted with methanol) to methanol in 10~l
volumetric flasks and dilute to the mark.b. Analyze together with samples and blanks (steps 11 and 12).c. Prepare calibration graph (peak area vs. mg analyte).
S/1S/BS 2004-2)
(Wf • ~ - Bf - ~). 1031C = • mg/m •
V
CALClJLATIONS:13. Detennine the mass, mg (corrected for DE) of analyte found in the sant>le front (Wf) and
back (Wb) soroent sections, and in the avarage media blank front <Bf> and back <80>sorbent sect ions.NOTE: If Wb > Wf/lO, report breakthrough and possible sample loss.
14. calculate concentration, C. of analyte in the air volume sampled, V (l):
fEASUREItENT:11. Set gas chromatograph according to manufacturer's recommendations and to conditions given
on page 2004-1. Inject ~le aliquot manually using solvent flush technique or withautosc1fll)ler.NOTE: If peak area is above the linear range of the ~rking standards, dilute with
methanol, reanalyze, and apply the appropriate dilution factor in calculations.12. ~sure peak area.
Method S255 for dimethylfol"ftllWnide was evaluated over the range of 11 to 61 eng/m3 at anatllespheric tl!q)erature and pressure of 23 °C and 761 nm Hg using a 4S-l sarple [1].8reakthrough occurred when a test atmosphere containing 119.5 mglm3 of dimethylfonmamide ~as
saR1)led at 0.859 Llmin for 146 min. The front section of the siHca gel tube was found to holo15 eng of dimethylform.nide under these conditions. The collection efficiency test conducted ata concentration of 61.1 mglm3 was detennined to be 1.00. Desorption efficiency at 0.759,1.518. and 3.04 eng per silica gel tube was 88.7. 90.4, and 92.2'1., respectively. A storagestudy for five days at 1.S mg dimethylfonnamide per silica gel tube gave a recovery of 91. 7'1..Overall sarpling and measurement precision, sr' was 0.056.
(1) DI~THYLACETMloe:and (2) DlMETHYlFORfWIlIDEfET.aJ: 2004
9. oetennine desorpt ion efficiency (DE) at least once for each lot of S1 lica gel used for~Hng in the calibration range (step 8). Prepare three tubes at each of five levelsplus three media blanks.a. Remove and discard back sorbent section of a media blank sampler.b. Inject a known amount (1 to 20 llL) of pure analyte or DE stock solution directly onto
front sorbent section with a microliter syringe.c. cap the tube. Allow to stand overnight.d. Desorb (steps 5 through 7) and analyze together with working standards (~teps 11 and 12).e. Prepare a graph of DE vs. mg ana1yte recovered.
10. Analyze three quality control blind spikes and three analyst spikes to ensure that thecalibration graph and DE graph are in control.
EVALUATION OF ItETHOD:Method S2S4 for dimethylacetamide was evaluated over the range of 18 to 105 mg/m3 at anatrll)spheric tl!q)erature and pressure of 24 °C and 760 nm Hg using a 45-l ~le [1].Breakthrough occurred .men satpling a test atnosphere containing 105.6 mg/m3 ofdimethylacetamide at 0.876 l/min for 240 min. The front section of the silica gel tube wasfound to hold 22.2 mg dimethylacetamicle uncler these conditions. The collection efficiency testconducted at a concentration of 105.6 mg/mS was determined to be 1.00. ~rption efficiencyat 0.943. 1.886, and 3.11 mg per silica gel tube was 88.8. 93.8, and 94.9'fo, respectively. Astorage study for five days at 1.866 mg per silica gel tube gave a recovery of 93.6'. OverallsaR1)1 ing and measurement precision, sr' was 0.067.
J
j
IIIIII
IIIIIII
I 5/15/85 2004-3
PETHOO REVISED BY: C. NNneister. NIOSHIDPSE; S2S4 and S255 originally validated under NIOSHContract alC-99-74-45.
REFERENCES:[l] ~tat\onof the NIOSH VaHdaUon lests. S2S4 (Di_thyla~ide) and S2SS
(Di_thylf~de). U.S. Department of Health. Education, and WlHa,., Pub1. (NIOSH)77-185 (977), available as GPO Stock 1017-033-00231-2 frca Superintendent of Docwnents.WAshington. DC 20402.
[2] NIOSH Ranual of Analytical Plethods, 2nd ed•• Vol. 3. S254 and 5255, U.S. Department ofHealth, Education. and welfare. Pub1. (NIOSH) 71-157-C (977).
Table 1. Pr'q)ert'es.
liquid ExplosivedeMity. BP ptp VP'25·C range in
Anabte g/ml @25 ·C 1:£1. ~ .!! !!!!1J!g ..B!! a; r! ,. vlv
oimethylac:etamide 0.9366 166 -20 170 1.3 1700 1.8 to 11.5
~imethylfonmamide 0.9440 153 -60 490 3.7 4900 2.2 to 15.2
Ir---.
IIIIIII,
(1) DlPETHYLACETMlDE and (Zl DlMETHYlFORMMlDE PET1()Q: 2004
IIiIIII!Jr"
I 5/15185 2004-4
APPENDIX D
ANALYTICAL DATA
28
-,
E.!. du Pont - 89-210O~STUOY
1.8
1.7
1.6
1.5
1.4
1.3
1.2
1.1r\•
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0.7
n6
U5
0.4
U3
0.2
0.1
0
0 2 4 6 8 10~
~houmts)O~, rrtiL
--
,/./U I,,""" i W~y~sl:,oYP
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tfI-( H.dd.. /JJOS/I ~t'-IPYt'#fC"e.. 2 co '!----=---------S;,.,ple ~ Ile~-hD·11f 0'
--L /Ht'~~!J~J''' u,iA.t ... r: / r ",/ S;~-htJ"': ,tJ.'~1II,2f!"j (J~
..2L. 7ic b~ / Typ< ..__~==:...;.::!J...;..:Ic:;.;.;&<..=--~:::;,. .;;.;~1:....- _
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LOCK ONLIJCK OH
'}
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)CiCi::ER 6,19:::9JJPCiNT DMF COMP~IANC~
l,:iMj 1:1. 53t·1M; SUPE;;Oi<;: o:;;:'THERMAL 1 tll;JC:1::T225.= INJ225~;;"HiE 11:'
G.5UL BLANK(WA7~R)
1
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"~ I) T ! ~~ E
TOTAL
C"~:OMATCiGRAM
~,Ai":~ll tlG ~~O PEAK:::-4,iK
...., -...., -':'0....,
:I0
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)
'00
)•-....,•>
~
....-..." (l'~-=;~=7r::;i~::~~':=0:,===========================11
e. ~~',
CHROMATOGRA~l
CR581 CHROMATOPACCrlANNEL NO 1SAMPLE NO El~~::PORT ~10 61
;:'KNO TIME
3.954
TOTAL49:::I~IPF'~ Dt1f
1(-=~,===.346====================
' • .i. .... :..
c;,,;,.c. ...
.:' .:.. '::'... , ._' '_' ....... f , ..
'.~ t'" .... •I :..: _ " __ :.._
::~581 C:HROMArO~~:'
':::-1AhriE~ ~'10
':; i=t ~1F' L E ,'I I)
,:;;C:;:'ORT t10
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•
C;iROMATOGRAt1
CR581 CHROMATOPACCriAtHiEL NO 1::;AMPLE NO tl;;;:::PORT NO E.4
r • L l
;1 Ci riLIli
p.nw TIME c u;~ C ;, '''''' i c..
)
TCTA~
! 2E.1:IPPt-~ Ii;-1F2762';' 1 i,:.i t':i
CriANtiEL t-JO'::Ai1PLE tiO:;:::PCiRT t-~O
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~
E9
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: !;,ll;.i
234646
C~~Ol CHPOMATOPACCr;~r-ir-~EL i-~O
TOTAL
---
! ''-''',,::;: . ::: :;:
TOTAL:26PF'M DMt'
'~
'J
]~.863( 4.958
CHROMATOGRAM 1 MEMOK:Z~D
CR581 CHROMATOPACCriANNEL ~iO 1SAMPLE NO 8REPOF~T NO E.?
F r Lt." £ TriO 11 282~
, 1:.
. ..TI ME
TOTAL63PPM Dt1F
2410: 11.:.J i.:J
3.:3624. '317
,,
i:; -: ~~ C! MAT CGRAr1
C~581 CHROMATOPAC::-iAN~~EL "iO'::,c,r'1PLE t'iO~~:':;:'O~:j 110
;<NO
:3.8E.2
TOTAL
C'-:":onATOG~:AM
~1852
l ... :.
'0o...
C~501 CHRO~ATOPAC
.. __,1_,, _
~ ---------TOTAL 188811
..
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-..
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...,
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n t.! ,,(J.1.1
AREI4 MK !J.lllU
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1 £11;.12,-..
52981-, :
Mt:~10RIZED
TP1E
3.872
Ci-iROMATOCiRAtl
3.886
CR581 CHROMATOPACCi-lAtiNEL NO 1
TOTAL
CC1~:or1ATOCiRAM
TH1E
3. '~26
CHROMATOGRAM
5. tl22
TOTAL 985':·TRAY 1 DILUTED 1:58
r';::: ~i C
HAY 8
C~581 CHROMATOPACCHANr.,EL NO:;;:H1PLE 1'10 £1
'EPO,,:T NO 71
HAY 12
CR581 CHROMATOPACCHANNEL NO 1SAMPLE 1'10 aREPORT 1'10 78
-
TOTAL
BOTTCIM 11:2(=):iJILUTED 1: 58
ChROMATOGRAM
.....:}I.,:,
_.-,
C~5e1 CHROMATOPAC,::riANNEL NOSAM PL E t-W (i
~E:PO~~T NO 7:3
TIME
3.979
TOTAL
~:2- I t~LET- I MP:
AREA ;1K il.i;'1C.1
7581~ S9877ni
75~:: :
'"'"..,o'"o..,'-l
o
-/ CHF~OMATOGRAI1 :1Er.C.I":I z£rr
CR581 CHROMATOPACCi-iAr'iNEL NO 1::;,H1PLE "10 (I
REPO,~:T NO 74
,- .-- I~l
c '.:.. L.. ..
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'0o..
•
"T;:::=----i~~.• ';14 1
5. 125
CHROMATOGRAM MEMORIZED
CR5G1 CHROMATOPACCHANNEL NO 1SAtlPLE NO EtREPORT NO 75
;-rLE
;"lE rHCil!
PKtW TIME AREA MK ... i'ilJ CUNC)
3.941 l'd572539rli
1 (11;.1
)
TOTALR2-rNLET-IMP2
1H57 )
I~===---""", ~14 65. 14
CHROMATOGRAM
C~581 CHROMATOPACCHAtit~EL NO 1~3At1F'L.E NO 8REPORT HO 7Eo
TI ME...,
":) •...,w
0...,0 --w.....0 ..
--0<)
0.. .~-...,..>
--.._-;
ED
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~tl "-'ll.......~
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.j
1';'1-, "
t ~ L.. to.
,1 i: l r-. (J 1.1
48364
4i~364 ::.
404~:hi
4.846
CHROMATOGRAM
R2 - I NLET '=:=li;i.l;:.:a....:W::!.)A SH
CR501 CHROMATOPACCHANNEL NO 1::;Ar1PLE NO [I
REPORT NO 77
J 3.9695. 131
~~2-0UTLET-IMP1
TOTAL ~
~
~
~~"'I
~
-_...
-)I1Ri'1t.
C:oC:.L
1U I~I
CONL:
f"ILlr·l£.THOil
A!'(:.R MK 11.111'.1
1 11EMOF~ r ZED
TIME
CHROMATOGRAM
PKNO
CRS81 CHROMATOPACCHAI'iI'iEL NO 1SAMPLE NO 8REPORT NO 78
--.
3.96'3 " 1 I~i <;.
1341ni
TOTAL~;2-0UTLET- I MP2
5. 14 Eo
o
CHROMATOGRAM 1 MEMO~IZEu
WARN I NG tiD PEAKR2-0UTLET-PROBE ~ASH
'" ..'"""0
4.842 '" ..0
""5.195 "0- "
CrlROl1ATOGRAt1 ;1EMCl~: I ZED
CRSB1 CHROMATOPACCHANI'iEL NO 1SM1PLE NO aREr:'ORT NO 79
FILEM£. r Hull
'0o...'"...»
PKNO TIME AREA MK 1 iJlI (I CL
".,-BOTTOM AFTER R2 DILUTED 1:58
JCHROMATOGRAM
5.187
1 MEMORIZED
.'
CR581 CHROMATOPACCHANNEL NO 1SAMPLE NO 8REPORT NO 88
tILEMET HOD
82821 - "
PKNO TIME AI<i:.i'l MK ~ lJ I) U t.:UNC i'lH,·Jt.
4.887 89887 ::. 1 UI;.,
18883hl--------- -------------
TOTAL 89887 HJG
R3-0UTLET-IMPl
"
4, 1~1~14
5. lE.7IV
CHROMATOGRAM 1,'lEMORIZ::D
-'
CRS81 CHROMATOPACCHANNEL NO 1SAMPLE NO 8REPORT NO 81
TIME
4.854
TOTALR3-0UTLET-IMP2
4,13445. 172
Ch~:OMATOGRAt1
CRS81 CHROMATOPACCHANNEL NO 1
ARE A ;'\ K ~ ~ ;'Il'
1491hl
F I d:i1E"1 HC.lll
c.: (J !'i C
101;.1
c: 1.:.1 "'" ..
...."") }.......
0....0 ~.......0- -'
-.J
-00...~)-......
)0-
-)
-)
ED
~-'
~..J.-)
--J
-,4.044 44 ~ .,:. -
TOTAL 441 ::::R3-0UTLET-PROBE ~ASH
4.0665.145
f,
.~
CHROMATOGRAM 1 MEMORiZED .,..,CR581 CHROMATOPACCHAt'lNEL NO 1SAMPLE NO E)
REPORT NO 83
TIME
4.866
TOTAL..R3-INLET-It1Pl
CHROMATOGRA~l
CR581 CHROMATOPACCHANNEL NO 1::;A~lPLE NO (I
REPORT NO 84
A~:EA r1K IDNO
1262·3
1122111
1262:;:
r I Lt.f1£YMUl.J
1 l:.J 1;,1
rIlEi1ETr-iLilJ
,', ~II'I"
'"'"...,:,'"0...'"~ .1
PKNO TIME CliNe (1 H(I t.0()
o... -'
4HI~I:::J.
339ol:.Jhl
TOTAL 41808.R3- I NLET- I I1P2
5.14
CHROMATOGRAM MEMOR1Z~D
1l:.Jl:.J
ltib
,
4.8131 42:301;,1272::.rll
llj Ij
) TOTAL
) "I
),~::::================oo""----------"""'~o2
5. 117
CHROMATOGRAM MEMORIZED
CR581 CHROMATOPACCHAIiNEL NO 1SAMPLE NO 8REPORT NO 86
FILE11 t:: -I H u lJ
F'KNO TIME AREA f1K 1 .... dU CUNC j"'I'1(il
4.882
18315hl
TOTAL
l'V ~
l'V -...0l'V0 .".........
'= ,.J
'00... J-l'V...» r,
...,~
~. ~
~1:I .J~..~
.J
J
2821rILEi1ETHOD
H~; t.. H n t\ ..... ,., II
::: ::: :.:: :.:~ ,.: .;;.
1 MEI10R! ZED
5.(375
TIME
CHROMATOGRAM
F' ,<ri 0
B;) TT 0 M WATE R 17: 113/~c)
CR581 CHROMATOPACCHANNEL NO 1SAtlPL E NO (I
REPORT NO 87
.•.
DUP R3-INLET-IMP2
, ....==----8.. ~ II
5. 13
CHROMATOGRAM 11EMORIZED
CRSB1 CHROMATOPACCi-lANNEL NO 1SAMPLE NO BREPORT NO 88
rILE.i1ETHOD
£12821
PKNO TIME AREA MK IilNO COhC
3.977 27561 ::;261nhl
'.
TOTAL 1 (:.1 I~'
':::===---";:::h. '~/' 1
CriROMATOGRAM
CRSB1 CHROMATDPACCHANNEL NO 1SAMPLE NO ~I
REPORT NO 89
'"'"w0
'"0w
"0-
"'00.... .II-'"....»
A' .• ,~' 4
-\
ED
~~
l
l --J,
N~ -
-\
t;,l
CLINC
r 1 '- t..
lit.. I "UI.I
MEMOR~~EDCHROMATOGRAM
CR581 CHROMATOPACCHANNEL tl0 1SAMPLE tiO t'~:EF'ORT t-1(1 9tl
TIME
TOTAL. 296B;::~:3-INlET-IMF'2 1:1 ~J/4988
296£18%28hl
R4-0UTLET-IMPl
JI;:==- ~: • 99 15.162
CHROMATOGRAM
CR581 CHROMATOPACCHANNEL NO 1SAMPLE NO (I
REPORT NO 91
rill.j"~Cj MUlol
PKtiO T1 ME
1 ::: ':, ... :::
1 'II)::; (, 1
cur1L
TOTALR4-0UTLET-ItlP2
4.00::'5.146
CHROMATOGRAM
CR581 CHROMATOPACCHANNEL NO 1SAMPLE NO (I
REPORT NO 92
1 1.:,11:1
,~ L .. E
'" -'" -w
0
'"0w....0-
PKNO T I tl E
4.888
H~:t.H 11K • <.'fl'"
2C:&::1
1 t:::': r. 1
...,o...'"...»
---------TOTAL
R4-0UTLET-PROBE WASH11;)0
CHROMATOGRAM
'"
PKNO TIME
3.973 66';06
85bhl
CUrlC
~ i,:,ll;'i
,
),
.."I,
TOTAL 66'nR4-INLET-IMPl
1 I;) lo
)
' .
CHROMATOGRAM
CR581 CHROMATOPACCHANNEL NO 1SAMPLE NO EIREPORT NO 94
MEMORIZE:D
rILEi'",E:THOD 2~12 ~
j:'KNO TIME CONC
3.995
TOTAL1':4- I tiLET- I MP2
t 5.044CHROMATOGRAM
584/:;;1
6681/tH
100
it , (' 1 tI
CR581 CHROMATOPACCHANNEL NO 1SAtlPLE NO 0REPORT NO 95
FILEi1t:TMl.lD
OJ
282.o..,o.........o
12186hl
TOTAL 89958R4-INLET-PROBE ~ASH
PKNO TIME
3.94:3
AKEA MK I~dC
89'358 .''00~-..,~
:l- ....
5.758
CHF:OMATOGRAM 1
CR581 CHROMATOPACCHANNEL NO 1:=; ;::. M P I I=" N n r,
.- ...,":' ...- ( .
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
•
2 ~1':' :
COI1C
27573ni
TIME
9%2hi
TI ME
3.971
TOTAL 882';'.:,
CHROi1ATOGRAt1
CR581 CHROMATOPACCHANtiEL NO 1SAMPLE NO 8REPORT NO 97
PKNO
TOTAL:BOTTOM 19: 1)8
F'KNO
(::-1 A lit! E L lEI::;;:'11PLE NO I)
;:t:F'ORT riO 96•
f
•••
•
••
•
•
•••
••
•
,
••
])CA PoVI-ltv~ ttJl S~ l'"YO j-~ ~1.- C~('-~C' T't"S'
A~'$t.. LG lM:.E/J..m.9
R,.{Py~~e.. 2e:t:> t./AHAJy:s/S ~t""_._D~M;....:.:.f _
~<#tl)d: Mo)tls;,.,P I~ ~ Ilee" "c;~ "_ /Hf/,I;'!J~'" 0' ~Ue"'~: ",1 S;~-h~~:
-X... ~,,~ I T'IP~" S; , ,'(g Gel (bock -vp to ;!1JP'~(~)
Dt-;6('1'h~H: VI) 4.~.. I. () N( ,§k,1t f.. metha '10/
~(? c,ltd;-f~DIf.s-"
/N';~C~'" 7';Nt," :/,)5 ''t' II(./~&-f(), l!lJ l4114~ : D. 5 tlRA'kcla.r hAttp: (~.;JS cst! .DC"~c.Io~ (Flo) l?4kl,:_'_D__
~4,- .. TyI' t' .. __5...c.lL""'f,p~e-:..(.:;.o~x_....Jko:!::::::-·-1-,'..:./.:.O...:m~+I_o=-';",:'S:..:3~,.I"\~fY\~;d:::-_
(10£<',.,.. 7';Hty: /J(I"I.~/: fa.; 0(' 7i;"'~ .. ;sc·tb('((l'\t\(~o
RQ H(, .. tt::'~A'"""If1Io:.:IH
,... IJA·r I;'Q./.. ~;._ T",Ht'.' -..;A4;.;.;.:.;;I"",;..
~~$.' -l:I..L
Co /I.~C:hD'" r;:'a I s...., tf I{~'h...f""..J;.,144J14 /J) 7i:"~ t,., ....) VO~(IAI) r";"c Aot"t'c"
stnd. ft;3D ppm 4·3'1 t 1311 115
"5tnd. I ~/I'J nnm 4.38fp ;)8, ;;'3Cf,
Sind (,,3 n~l'V"\ 4.44B 15,11j, ,
Du 1> : sind . '"3 n.:> rt"'l 4,387- 13 q41
000 (7.): Sfnd .~!M 4.45/P 15 07:1, I
~Vl'\ l i~'td, Front N.D.
Run 3 , I (\ \ et, tro() t tJ. D,
l..J 1,\ pC,.J' I , U' I r an£) "I .) l.j
boc K- ·u P tu be',)
--
sqltf"/~t:'. lice />,. .. F,......' sa-I/~ Il, frlCfa'llA
It> T,:'~ l"':M) v.-..., (_I) 'T~"""'~ A"t'A
"t.( t'\ 4 inlet Front kI.o.SPI rc::"6: "3 p p rtl "5tnd
4.3~q 4;)00RUl1 2 i nlpi fnm~
~PIKE ~ I~'" ppM 5ttld.Ru~ 2 ,~Ie+ kv~t 4.340 /0 181
Run :J OlAM trun1- N,D.
Rt..\o 3 £jI.(Het Front fJ· D.
iltJf'l tf ovt/d ~f'\t N·P.
i\~~~~
""~""""'"""~
'\
I"-~
'"'"~,,
.' '. .. ~ ~. :... ri
13/9/89 DUPONT DMF R~~~Y~~~
.:.• ; "-:A GE ~ iF' 'r I.''':;::'':,
)
,.;; " ,j ;., •.. ,.; :::
., .
c.J
I)
o42821188
L--===============- r-,. :;:'~,-'
D'1; SHi[l-638PPM
ATTEh;~::THOD$
SPL.WT
.j: DT H
D~IFT
~.DBL
L:"';~Oi1ATOGRAt1
S~581 CHROMATOPACCc'Ar~NEL !~O
TP1E
1 • : 03 -' '-"1.. ........
1.371
4.397
.:. 0.' .....:. '.~I... ( ,. ,.,.~
...~' - " ..:
.:. ( • I....I( ...
- ,J
TOTAl.:l··~:'" ::;T~1D-126?pr~1
'"'"wo...,ow....o
:: .. =:O~1ATOG~AI1
~~501 CHROMATOPACCriRNNEL liO 1
D2
'"...>
)
..
.., ... '.' -.•• •••• ~ 1_; T I 1'1 E
4. :3:36
,., .., .~
4.44 :3
) CHROMATOGRAM ) .
• I
.)
CR581 CHROHATOPACCHANliEL NO 1SAMPLE NO eRf:PORT NO 3
TIME
4.448 1577/182?hl
fiLii1 t::f H LI JJ
., .
.'.TOTAL : 5777
::.iP: DMF STND-6~:PPt1
)
-,
CR581 CHROMATOPACCriAliNEL tiD 1~; H;,- F'L E :'1(1 £I;:::;:'OF;:T NO 4
r" ~ L. ~
j'; t: Of i'1lJ JJ
A"': ::.. H '~ ~::, .. '-' :1 '_.
TOTAL 1 :3',4?DJP(#2)-DMF STND-63PPn
1 MEr10RIZd'
'"'"w0
'"0w.....0-
-,'00~ I-'"~> -,
-,(B
~......J
J,
r J. L:'
f1t. 'j HUli
1 b 1';'1
CHROt1ATOGRAI1
4.387
T I 11 E
CR581 CHROMATOPACCHAIHiEL NO 1SAl1PL E NO 8REPOF:T tlO 5.......;
COJIKODBALTH 01' Vl:RGZBJ:ADepartJIut of Air Pollution Control
ZI1TRA-AGDCY IIBKOUNDUX
TO: File
I'ROK: R. o. Goetz
SUBJBCT: DUPONT, WAYNESBORO, REGISTRATION '20517
DATB: November 2, 1989
RE: STACK TEST •••••EW DMF SCRUBBERS ON ORLON FIBER DRYERS
A witnessed stack test was performed 10-31-89 on one of two('1 scrubber, away from river) new large scrubbers for DMF (VOC)scrubbing efficiency, inlet and outlet concentrations and poundsper hour emission rates. The scrubber tested was fully loaded(one-half scrubbing capacity) by full production on one-half (3)of the six orlon fiber dryers.
Opacity appeared to be zero (0%). It was impossible to besure this date due to fog the first two test runs and a cloudybackground the third of three test runs.
See the attached stack test monitoring sheet and proposed testprotocol by ETS for more details.
- "Preliminary" results indicate better than 95% DMFcollection efficiency, less than 5 lbs/hr DMF emission perscrubber.
DMF concentration in scrubber water reservoir: 3%. Planthopes to increase this to 9 or 10% for more efficientrecovery.Inlet feed water: 5300 lbs/hr -- 11 gal/min.Ran about four days before test day.
\
• .I. . SAMPLIIG POlft LOCATIO.
NEXT31-0CT-B9 14:38:20
sall1 LIQUOR FLOW€8i3 L?/HR
':;)00,00 i \i I I, i! iI i81,OO'11T'-m-tt---tt-tTt-++U----;-ll-~II I3601),{j():-rft1-tn---fTffirftf-+--\-hWJJi-.-J! i i
~'40~'OOi1ilttltt-frtf+-+4~~41-~Uj-~~ . I
It i2A.oor!.......Jf~n-n+lf-+i-~-+---IJ---:1 I !\ll-----.J ILJ ,.,)~(;O 0.or.ll--IJ3(r:'='--L~-~r:r-!..--l_-- I'1030 ..31-OCT-89 133~O-------L--~--1500
WALLACE E. REED. CHAIRMANCHARLOTTESVILLE
TIMOTHY E. BARROW.VICE CHAIRMAN
VIRGINIA BEACH
SAM C. BROWN. JR.VIRGINIA BEACH
RICHARD L. COOKRICHMOND
MANUEL DEESERICHMOND
WALLACE N. DAVISEXECUTIVE DIRECTOR
COMMONWEALTH of VIRGINIADepartment of Air Pollution ControlVALLEY OF VIRGINIA REGIONAL OFFICE
SUITE 0, EXECUTIVE OFFICE PARK5338 PETERS CREEK ROADROANOKE. VIRGINIA 24019
703 857·7328FAX 703 857·7snTOO 804 371-8471
October 16, 1989
DONALD L SHEPHERDREGIONAL DIRECTOR
Mr. Ron ShifflettE. I. duPont de Nemours andCompany, IncorporatedWaynesboro, VA 22980
Dear Mr. Shifflett:
Our review of the of DMF removal efficiency ofthe and the test report you submitted has ledus to cone ude a~ I; thecapability of this ~sign to remove ofcaptured DMF. In conjunction with your earlier emissionsinventorying and stack testing that indicated that approximately77% of plant DMF emissions are exhausted by the stacks nowcontrolled by these scrubbers, we also conclude that the 69%overall OMF reduction target specified in condition #15 of yourJuly 3, 1989 permit has been met. You may therefore start-up thenew Lycra spinning equipment described by that permit.
You are reminded that you •••.......... in order to comply with condition #5 andwith the remainder of Condition #15 of th and thatconditions #6 and #16 must still be met by April 1, 1990.
Please feel free to call if you have any questions.
Sincerely,
~;z'r~~Donald L. ShepherdDirector, Region II
cc: ...
it-nODI-We
<M)POBJ)..r.tJ"_._~
WAYNESBORO PLANT
WAYNESBORO, VIRGIN'IA 22980
TEXTILE FIBERS DEPARTMENT
October 10, 1989
D.C T1 2 1989
Mr. Donald L. ShepherdDirector, Region IIDepartment of Air Pollution ControlSuite D, Executive Office Park5338 Peters Creek RoadRoanoke, Virginia 24019
Dear Mr. Shepherd:
On Fridon ourplant. The compliance sampling was performed by ErS,Roanoke, Virginia•
. Prior to the start of this test, we were requested to provideinformation about certain measurements that were to be taken duringthe compliance testing. A copy of that requested information has beensent to your office. You also requested information about the ORLONproduction rates during the testing. This production information was notincluded in our recent submittal due to our opinion that it is
Below is the information that you requested.
TestNo.
2
3
4
StartTime
11:26
13:47
17:17
FinishTime
12:26
14:47
18:17
DryersOperating
12, 13 &15
12, 13 & 15
11, 13 & 15
Pounds ofORLON dried
15,928
14,845
14,981
I would request that you treat this information as confidential.If you have additional questions call me at (703) 949-2844.
Sincerely,
~G3.~ft!Ronald B. ShifflettSafety, Health &EnvironmentalAffairs
CO"T" ..... ~ "(~. T '-T "l... .". ~ . ' .• ,'" t·, < •.4 .. _..., ....... • ~._ ...!.. ...........
L
COIDIOnBALTH OF VIRGINIADepartaent of Air Pollution Control
INTRA-AGBNCY MBKORAHDUX
TO: File
FROX: R. o. Goetz
SUBJBCT: DUPONT, WAYNESBORO, REG. NO. 20517
DATB: October 16, 1989
RE: STACK TEST NEW DMF SCRUBBERS (ORLON)
A stack test report has been received for the October 6, 1989stack test of the new no. 2 (near river) DMF scrubber on orIonfiber drying. The test was witnessed by R. O. Goetz with S. K.Barnard observing opacity (always O%).
The test report showed that this scrubber was "in compliance"with an efficiency exceeding 90%. It averaged 96.3% efficiency forthree test runs.
The scrubber was fUlly loaded by all emissions from one-half(3) of the dryers at capacity venting through one-half thescrubbers (1 of 2).
This test is in J;eference to the July 3, 1989 permit forseveral areas of the plant and a related consent agreement.
There will be a similar test of the other scrubber in a fewweeks.
For additional details, see the test report and 10-12-89 memoof test observations.
~.o.~RaYmond o. GoetzEngineer, Region II
ROG/bh
Attachments
CC: DI£"5,1<. BARI\AR'O
