Document a4B3x8jyv76bQw83x772YKm1a
ETHYL CORPORATION Medical Department Baton Rouge, Louisiana
STRICTLY CONFIDENTIAL
INDUSTRIAL HYGIENE SURVEY of
Baton Rouge Plant
Preliminary Survey of Materials and Processes in
PVC OPERATIONS
I. General
The sector of the Ethyl Baton Rouge Plant designated as PVC Operations is principally involved in converting vinyl chloride monomer (VCM), produced by the Hydrocarbon Area, to polyvinyl chloride of both the "suspension" and "emulsion" types. The area also produces a special oxygen-barrier type resin (Barex) for Sohio under contract.
A simplified lay-out of the plant is attached as Figure 1. This plot shows the Reactor Building, with its batteries of kettles, and also designates the areas for finishing, compounding, and warehousing. Figure 2 provides a simplified flow diagram, beginning with monomer, and showing the finishing stages of the "suspension" type resin. Finishing operations on the emulsion "resin" are shown in Figure 3.
Three lists of materials, originally compiled for various purposes, are attached. These are being reconciled into a common list, and MSD sheets are going to be available for most of the items. (A substantial revision of the lists has been necessitated by a recent switch of items in the product mixes of the Tiptonville and Baton Rouge plants). A fourth list shows raw materials used in Barex manufacture.
For present purposes the operations may be divided into five areas: Polymerization, Suspension Resin Finishing, Emulsion Resin Finishing, Resin Compounding, and Barex Resin Manufacture.
The writer had the benefit of a briefing by Henry Smith, Superintendent of these operations, and also of Wilbur Paulk, Mike Hopkins, and George Johnston who guided me through the various parts of the plant. Bol? Callander described the Barex operations.
EC 4263
II. Principal Materials (Raw Material, Product, By-product, Supportive)
2
The materials mentioned below are only illustrative. the attached lists show, hundreds of materials, including dyes and additives, are used in producing resin products. A large fraction of the products are produced and/or compounded to customer specifications. And many of the polymerization recipes themselves are proprietary. Accordingly the following sections of this report are intended to serve simply as a rough outline and guide to assist an in-depth study of the situations with which the hygienists need to become familiar.
As
Suspension Polymerizations
The-suspension polymerization kettles are designated with an (s) in the circles at the left of Figure 1. Those
four in the cross-hatched lower box are newer and larger vessels.
Most suspension polymerizations are run at pressures above 100 psi, ranging to about 240 psi. A typical reactor charge will consist of:
1) Suspending agent, e.g. "Alkatex",(polyvinyl alcohol)
2) Catalyst, e.g. dodecanoyl peroxide, or X-16, or both. X-16 is a proprietary catalyst prepared on-site._
3) The charge of vinyl chloride under pressure
4) Antifoam (silicone)
5) Short-stop, e.g. para-benzoquinone in chloroform
or acetone.
----------
The kettle is heated to begin the reaction, but chill water is then circulated to absorb the reaction heat.
Emulsion Polymerizations
These reactions are usually run at lower pressure, e.g. 100 psi. A typical charge will contain:
1) Emulsifiers. Various soaps, (all purchased). Calsolene TlCI), a sulfonated oleate. Myristic acid plus ammonia. "Sipex" soaps. Triton N-361.
FC
2) Isopropanol
3) Anti foam
4) Vinyl chloride charge
5) 10% ammonia or 1% ammonia or 25% caustic (Allied chemical) for pH control
6) Shortstop, e.g. benzoquinone in chloroform or acetone
Polymerization Operations - General
Chill Water. Water is cooled by two Freon-11, and one F-12-charged units for use around the jacketed reaction kettles, and also to cool some solution make up tanks.
De-ionized water is required in the polymerizations. Water from drilled wells is de-ionized in:
3 cation exchangers 3 anion exchangers, and then 2 mixed-bed exchangers
The beds are regenerated by caustic and sulfuric acid.
Vinyl chloride recirculation. The flow diagrams trace the movement of VCM. After a polymerization reaction is complete, the kettle is depressurized, then de-gassed under reduced pressure. This unreacted fraction of monomer is sent to the holder shown in Figure 2. The stored gas is compressed and fractionated in a stripper, where the non condensables (mainly nitrogen, with some monomer) are vented. The condensed monomer is returned to the storage feed tanks. (An incinerator is planned for disposal of this waste).
Suspension Resin Finishing
De-gassing. The slurry of resin is discharged into a de-gassing tank (see Figure 2), where vacuum pumps boil out the reacted monomer, by-product gases, and atmospheric gas (essentially nitrogen). These flow to a gasholder. The gases are later compressed and the non-condensables stripped out and vented. (See planned incinerator).
Centrifuging. The slurry is centrifuged to separate the suspension resin from the mother liquors. The resin drops into a rotary dryer. The aqueous effluent has a generally clear appearance, and appeared quite free from odor. It contains all the chemicals which do not enter the reaction, of course, plus by-products. This water is discharged into a sump and open ditch leading to one of the ponds. No analysis was available.
4265
4.
Drying. In a rotary dryer, the resin is blown with air filtered and heated by steam (from Gulf States Utilities). The moist air exhaust is discharged through chimneys on the roof. Besides water, the discharge contains relatively low proportions of VCM and other organic volatiles. (The moisture shows up in the form of fog on occasional winter days).
Emulsion Resin Finishing
These operations are shown in the diagram of Figure 3. Emulsion resin particles are very much finer than suspension resin, with size in the range of 30-50 microns. (These products are intended mainly for shipment as the powders to purchasers for use in making battery separators and many types of coatings.
Drying. The emulsion from the autoclaves passes through screens to 1) storage tanks to 2) pumps feeding the 3) spray dryers. In these dryers, filtered and steam-heated air flashes off the water scattered by a spinning disc. The powder is dropped out and conveyed in a blast of filtered air to cyclones which separate the product and drop it onto screens which reject oversize particles.
The air from the cyclones contains some powder, and this is removed by dacron bag filters (500 bags). The air is discharged at the roof. (Since no liquid was separated by centrifuging or filtering, the discharge air from the emulsion dryers contains all the water, as well as all the volatiles from the polymerization process).
(Occasionally a bag bursts and a cloud of resin
powder billows up at roof level. This event is not
monitored by equipment, and is detected only when
someone catches it by eye).
__
The product passing the screens goes to bagging equipment.
Grinding. For some purposes the finished emulsion resin is still too coarse, and the product is fed to a grinder to produce a powder which meets customer specifications.
Resin Compounding
Most of Ethyl's PVC compounding operation uses suspension resin. (Supplies of the resin are kept stored a silo. For any particular recipe a weighed batch of resin is mixed with any of many varieties of dyes, plasticizers, processing aids, etc. (see list at end
this report) and fed into a ribbon blender. (Most
of the additives are received in bags or drums). The mixture goes to a heater, and is then formed into hunks, or "bricks". These bricks go to a roll mill, where they are formed into a sheet and then cut into strips. The
strips are cut into "dice". Shipment is niade^in'^ags7^ large boxes, or 180,000 lb. capacity rail cars.
in
EC 4266
Darex Resin Manufacture
Ethyl makes Barex for-Sohio under a contract with limited term. Sohio is now building a Barex plant, and they have licensed a Swiss company (Lonza) to produce the resin. Much of Ethyl's product is shipped to Vinyl Plastics, Inc., who extrudes a packaging grade film. Oscar Mayer is a principal customer for this.
As many as 28 raw materials go into Barex manufacture. (See attached list.) The process is complicated, and involves several steps. The recipe calls for a number of pre-blends to be made up.
In principle, Barex is made by preparing a nitrile elastomer latex which is stored temporarily for use in the second step. In the next step two other monomers are grafted onto the backbone of the elastomeric polymer. The final product is coagulated into short, white strands, and is shipped in this form. Much of the process information is proprietary, and for industrial hygiene purposes it should be necessary here only to identify the raw materials and understand- their roles in the operation.
Nitrile rubber latex. A soap is prepared from Emersol fatty acid and potassium hydroxide. Other ingredients:
Stabilizers and Antioxidants Polyguards and Naugards (Uniroyals' Nos. 401, 402, 403, 404. MSDs on request through Sohio. These substances remain in the product).
Catalyst, dry: DuPont VA 20-64. Monomers:
Acrylonitrile (tank truck) Butadiene (tank truck) Chelator: Versene Daxad Tertiary dodecyl mercaptan
This operation is conducted under pressure at slightly elevated temperature. Two or three batches can be prepared in one day. The 6 batches from 2 days operations ("one campaign") are adequate for making 40 to 60 batches of Barex resin, and are stored for this second step.
In the second step acrylonitrile and methyl acrylate are grafted onto the elastomer.
Other ingredients:
Qtas8.ium persulfate. (catalyst) Mercaptate Q-43 (Cham transfer
agent. Injected as reaction proceeds) (Obtained from Evans or Carlyle) Polyvinyl pyrollidone Monowet, as emulsifier. Also Gafac.
4267
5.
After 6 batches have been accumulated in the second (qraft) step, these emulsions are coagulated by the addition of an alum solution. The mixture is next extruded through a perforated disc into water kept at 180F, forming single wrinkled strands, roughly one inch long. These are screened, washed, screened, washed, and finally dried.
By-products. The autoclaves are de-gassed under vacuum, and the exhaust vented at the roof. The major organic effluent from the latex operations is butadiene.
6.
About 85-90% of the monomers used in the Barex plant goes into the product. The waste water from the first screening is hauled away in tank trucks by Rollins Environmental (Div. of Rollins International). This liquid contains a lower aqueous phase containing about 5% of unreacted monomers, and for disposal is biologically treated. The upper, organic phase-mostly monomers plus low polymers-is burned by Rollins.
The exhaust from the final drying of the resin contains some monomer vapor.
The wash waters (produced after the first screening) go to the ditch. These contain some Monowet, some monomer, and some of the resin.
III. General Notes
1. Waste PVC. The plant produces considerable material which is either particle oversized, or suspended in effluents, or below grade. Where possible, the offgrade and off-size material is sold. Floor sweepings and other solids go to landfill. Large amounts of material accumulate in the settlings of ponds. The ponds are periodically drained, and settled wastes hauled to landfill.
2. Autoclave Clean-up. The walls of the PVC autoclaves are purged with high-pressure water after every resin batch is discharged. The wash water flows to the ditch and pond, carrying PVC scrappage.
Attachments: Figures 1 to 4 Lists 1 to 4
D.E. Cooper October, 1974
FC 42A8
PC A2t>^
EC 4 2 7 0
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EC 4272
MATERIALS used in COMPOUNDING AREA*
Serial Series Code (see list in following pages)
0001 1000 2000
3000
Supplementary polymers
Plasticizers
Fillers (modify opacity, color, wear, etc.)
"Special", esp. fireproofing agents, etc.
4000
Stabilizers
5000
6000 7000
Lubricant additives - internal and external
Pigments (organic and inorganic)
Impact strength and modifiers
*This list is partially obsolete, and needs both additions and deletions, due especially to switches in Tiptonville and B.R. product mixes.
RAW MATERIALS AND MISCELLANEOUS SUPPLIES - PVC AREA -
/ y/ *
A/*
' X*$* S'**?
Cp^c
\
Name
OGU
Styron 685-26-7
0012
Tyril 867-21 Natural 7
1008
DOP
1013
DIDP
1023
Drapex 4.4
1026
Cerechlor 42
1028
Cerechlor S-52
1079
Santicizer 160
1083
DOA
1107
Epoxol 7-4
1175
Epoxol 8-2B
2019
Celite 263
041 Atomite
2042 2047
Winnofil S
*
Onyabsh
2054
Fiberglass
2055
PPG Fiberglass
2057
Desertalc 57
2058
P-414
2059
P-413
3147
Jayflex 205
4009
'CH-55
4020
Advastab E-82
4021
BC-103A
g|25
TM-303
State Soli cl sol; | `,C|UlA
ChemJ.cal Composi11 on
sAy V't'nc. 0-C.vyt O rv>4" y >\<t pol yvx-.e.
s4y rc*\_ OC'ry l5 *vA Ylc ^olyWvrv-
JU - re4Uy/ koty f plvP *\C (afc_
1 ^\ <^LM
\ l<\ U.. (5-
\;^;A
I A\*ju. I
* li^`A
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A\^u-< AK^u.>
t - Z*
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fiCV^CL Ot }
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4032 4035
Tinuvim P Mark 356
*
^O.'T .
*
Q'
FC d?j4
?\W MATKKMJ.S AND MISCEI.I-ANKOUS SUPPLIES - PVC AREA (cont'd)
Code 4049 4056 4063 4081 .4086 4088 4113 4114 4115 4129 4130 4142
154 4156 4172 4200 4210 4211 ' 4219 4220 4221 4223 4232 ... 4233 5006
018 5023 5027
N^uie Mark C Mark WS Mark OHM Cardinal No. 1 Cardinal 10 Cardinal 2 AYA Cardinal Clear 54 Mark 152 Mark 577A Irganox 1076 Ferro 1827 Ferro 904 Scotch Laddie 810 Scotch Laddie w/Kaydol T-31 DiBasic Lead Stearate Tri Base EXL Synpro 530 Mark 417 Tribasd. LPC Plastiflow LPC Mark 734-A Irganox 1010 McGregor 918 or Scotch Glyco RP Acrawax C Aldo MSD Wax E Powder
State
sol So\*l \\
__Chemical Composition X'So-QC'Vwy (ykos^k.-lc_
Co<0mv.`.o^--/ pavt\-o*-y4t\v +o\
V\s0&`sQlej&
Oa&r*'
a; bu4^V,^ dhU^^t-
\; ^T'O^T . flA`CL>rM 4*' * i U 1 *
CrjAcA ul^w ^ i
5
& CCL$d|
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6
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+ -, baSiC |e.aj^
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'Vkl a ^\y c 0 f^
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5o\* A*
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v U>v*> (kaJUr*
1 *v*C4^ ba S / c. I d-Qu^
ie~ac$- a^a.JLWflct'C. |u(sr
ha -C-OLdOv^S -* $uk4*t4vo|-u5 (J
\ Y*\\jCLS 1 C y ttraf
Ucufi. QjkHxa-U-4-e-. v c \ 0 \ <-C*-4 C_
Va.'s 5"f'C.av-v^*^<l ,'V^n'^^"cv>c-
<o(xy(LA''r/ wser^O fiVto-vdltC,
VAO^'^ G-'Vn. ^4-^6
pQ 4?75
LAW MATERIALS AMU MISCELLANEOUS SUPPLIES - PVC AREA (cont'd).
Code 5028 5036 .5037 5044 5047 ;5051 5059 5064 5066 5068 5073 5075 6002 6007 6008 6010 6011 6012 6014 6015 6023 6025 6026 6029 6030 ^^6031
6032 6035
Name Wax OP Flakes Calcium Stearate Stearic Acid Aldo M0 Aldosperse 0-9 Kaydol Sodium Stearate MS-2 Resin Aldo S-932 Wax PA-190 Advav?ax 165 629 A Wax UB Blue 59-4967 .Lakeoline Violet 1
t Apex 8003 Aluminum R-500 or R-100 R-101 RT-791-D Violet Ti Pure R-900 RF-1 or RF-2 FDC Violet Drakenreid 1C324 Sun Yellow Sea Amer 1162 Yellow Amer 1166 Yellow Amer 1167 Brown Amer 1198 Black Amur Yol low 1206
State So\ * A So\\A
Chemical Composition S^nvN>,Cl\ f il V'^er'i-iVo-v^
^>o\^ oHq yN--n \ v\ e. e-O- (
i o\e-d-V<^ r^tr^o- oWc
^
e^i-cr^C- *\V\t4 av>-L
avNsteft'c* ujclx
eoUcS-
>cA
\%
401.
soua
sd :i
V v eft >oU<&
^araP^v, Vy^oc*T-ker~
(&*<_\ r ____ ^vVc*-4<-
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a, Sol~t-
p o e e
w\ n y*\ u
it
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.
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?C 4276
*V' Lf-KiAVj^ AINU MISCELLANEOUS SUPPLIES - PVC AREA (cont'd)
Code 6036
Name Amer 1204 Yellow
6039 6040
1484 Maroon
*
X-2'541 Yellow
604%4
6045
M.B. 1049 Black Amer Orange 1026
6046 6047 6049
Amer 1050 Blue Amer Yellow 1056 1058 Green
6050 6052
IMP X-2944 Perm. Green FDC Green 1100
6054
3300 Blue 18
6060
Reynolds 50 Paste
k6064
14-4008 Hosta Perm.
6071
Raven IS Carbon Black
6072
Molacco H Black
6075
UMB Blue 4725
6076
Tinapol PCR
6077
10369 Brown
6080
UB 0008 Violet
6081
V 5100 Dark Buff
6082
Ferro V-5101
6084
.X-2155 4..1Yellow
6085
10380 Grass Green
6086
X-2315 Deep Yellow
6087 0P89.
X-2272 Primrose 11 RjJjQacjJS-Red
6090 6091
R-10-3C 114-CTl`gTTae R-1-Q-3G--113- Orange
State so\~A o\ v*S S6 \ v(S. So\`A soCA .so V r & s.ui ^o\ * JL
& o V \ <4
QasVe-
eoWJt
Chemical Composition
C,Uv A^O 'C-- Vr`*A
i
cV\V- trvo. o>-
''4'ClvT
i
^
r o"wv v tow* olfi-V* t v<f^ i U
c_^ *>. o-rv- 0 34*^^-
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fl.luv^Vui--/vw
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sol . sa V \ A
5 o W cfi.
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^>o\ \ A
Z>o \ .
5o\ itP
3 V i
5o\\
5o \ I &
5o l .
50 1 $
M "L X^CT-v^ V\y Ar 0^ Vm-30^ ^ c>^rtC
J3tNr;0a+;vc
*ob5W+<l it I* EC 4277
\w LNAjr.KJfU.s and HiSCKI.lANEOUS SUPPLIES - PVC AREA (cont'd)
Code 60% 6096 6098 6103 . 6104 6107 6109 6!iA 6118 6120 6323 6124 ^126
6127 6128 6129 6131 6134 6136 6138 6139 7002 7003 7071 ^072 ^^001
8002 8017
Name
State
Chemical Composition
Monarch 74 Black
Violet ZIRS YT `5621) Green Gold V-5102 Brown
>o\ \ A
50\\&
FDC Violet 1 Drakenfeld 10383 Ky-7SSD K/-781D Amer 50 M Red /3Z? ft. \
>o \. A
t>o \ A
50 VA
5 1; A
Drakenfeld 10382 Brown Mapico Tan 15 Mapico Brown 421 Mapico Red 477 X-2925 Monark Blue g
so\A *eV><Q so v; A. 6\ \<A.
YE 42 ID Orange
S*t>\ v l
Y-469-D Yellow
-------------- - 5o \ i S-
Raven 30 Powder Cromoplital Yellow 3G Tone
to\ c A 5o \ i A
C-kro~r^N >' **-*'v\.
Ctatro-rv'N % /i
I'i** --C. /^\4'
0-J,O i C_
C.UvO-ws i W-
<m o ti
C i
I4
pV^aV ocya
v-err^ * u'v%'~'* --j--^<2 V* \ v/o'l' I \J
Ti02 Cr 800 PG Amcr Cyan. Blue 55-3750 KR-980 D K-120N Blendex 575 Nevadinc LX-509 Piccclastic D-125 Blendex 301 Blendex 401 Blendex 311S
6ft \`\&
*
\0 C^Ct ^ ^
so\ r<JL yv\0\y h>Aakc-/c.Vv~C"Vv''
*d\' *o\'.<St s*eV\4L
o.<^;c- ($'>''i'"'' OC.rJo.vW.'c -
4
v C,u-V^A *>'rtrvNC- \
6 14
ScA' A
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Soi;fi
*
5oV*'A
5 u
, T-(J^
*i
A
FC 4278
Product jfan
Adogen 58
" /
~r ~ ~'i Supplier
Ashland Chemical Co.
Advastab T-340
Cincinnati Milacron
Advastab TM-181S
Cincinnati Milacron
Alcotex 72. 5L
Revertex, Ltd.
Antifoam 60
General Elec. Co.
Barium Stearate Blend ex 436
Snythetic Pr. -Americhem Marbon Chemical
Butyl Benzyl Phthlate Hatco Chemical BBP
Butyl Stearate
Emery Industries
Butyl Diol 1, 3
Celanese Chemical
CPE 3614
Dow Chemical
Cadmium Stearate
Synthetic Products
Calcium Chi. anhy. reagent 12 mesh CX 150
AWC, Inc.
Calcoline Oil H5A
ICI America
Colloid 987
Colloids, % Chem. Soln.
Ccpper Sulfate pent. McKesson Chemical
Dibutyl Tin Laurate
Cincinnati Milacron
Dioctyl Adipate DOA
Monsanto Chemical Eastman Chemical U.S.S. Chemical
Di-bnsic lead stearate National Lead Co, DS-107
Dioctyl Azelate DOZ Ashland Chemical
Dioctyl Phthlate DOP Ashland Chemical
Drapex 4.4 DM-7704
Argus Chemical Co. M&T Chemicals
I
Product
Supplier
Electrocarb 105
Hammond Lead Co.
Epoxidized Soya Oil Ashland Chemical
Epoxol 9-5
Swift & Co.
Glycomul L
Glyco Chemical
Clycosperse 05
Glyco Chemical
Kane Ace B-18A1
Mitsui & Co. Kaneka America
Kane Ace PA-11
Mitsui & Co.
Kaydol Mineral Oil Witco Chemical
LX-509
Neville Chemical
M&T T-66
M&T Chemicals
M&T 7888
M&T Chemicals
M&T 8494
M&T Chemicals
Mark 152
Argus Chemical
Mark 417
Argus Chemical
Mark 734A
Argus Chemical
Mark 971
Argus Chemical
Mark 292
Argus Chemical
Mark 1911
Argus Chemical
Multiflex MM
Diamond Shamrock
Myristic acid 1499 Kortman & Schultz
Parabenzbquinone
Eastman Chemical Pr.
Pluronic L.-62
Southern Solvents
RE Titanium Dioxide New Jersey Zinc
Synpron 1115
Synthetic Products
Synpron 1314
Synthetic Products
Snypron 1169
Snythetic Products
AS*'^ ^ Rec'd
t/
V
--
80 4 ?80
1
Pproduct______________ Supplier
RT-791 -D violet YE-421-D orange
E. I. Dupont E.I. Dupont
Y496-D yellow
E. I. Dupont
K0786-D Kroler orange E. I. Dupont
Y-488D Yellow
E. I. Dupont
V-5102 brown
V-5100 dark buff Drak. 10383
Drak. 10324 amber brown
Ferro Corp. Ferro Corp. Hercules, Inc. Hercules, Inc.
Imp. Red X-2327
Hercules, Inc.
Primrose yellow X2272 Hercules, Inc.
Kristalex 3085
Hercules, Inc.
Lakolene violet #1
H. Kohnstamm
Iron Oxide brown 420D Reichard-Coulston
SOM violet cone. 1963R1- Synthetic Products
Ultramarine blue 495 9-00 Whittaker, Clark, Daniels
u282
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t
FC
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CODE
1,11....
COMPOUND
MAXBBZALS
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r t&3t>w r 1 e *<n
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ypvu StjojPilon 1003
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