Document jmG0r46OGw3ka6p3v26YB4XVR
'.'.CO* A. C. Huiston
. S. -A. Salvage
fc. N.* Shiipley
Vv`,,:
H. N. Ta>ylor
Pile: 81-9
TO: R. P. ANDERSON
' '
..
August 31 19*66.
r
PROM: R. O. ALSUpR
1. '
*
r
DISPOSAL OF SOLID w3TEFL0NltWASTES CONTAINING C-8 APPfC 1 '.
Introduction
,.
\
Some of the soliids wastes from the Pine Powder a m d ` Dispersion Area of the "Teeflon" plant contain small amountss of toxic perfluorocarboxyllic disprsing agents. A cheap aind ... acceptable method of dispensing of these solids is in a lamd fill, provided that the; tcoxic agents are reduced to an accept able level. Since th disspersing agents are volatile at moderate temperatures, we set out to determine the conditicons necessary to bake the res'ilns to a non-toxic state ;
Summary and Conclusions:
" ..
1. The dispersing agent level di* the solids waste stream is reduced! to a quite acceptable level (below 2 ppm) by baking at 175C for 5 hours.
./%:
2. Without a pretreaatment, a small amount of the perfluorocarboxyllic acid dispersing agent would be leached into tfche ground water.
'
Discussion:
*A system for colLlecting the solid wastes from thee
Dispersion and Pine Powder? Area was proposed by Anderson amd ,
Chren. This involved the use of sumps and settling basins to
concentrate the solids. SJolids in the form of coagulura frcom
wax filters and wax separator settlings were also to be coILlected
in this system. A flow shieet of the proposed system is atttached.
The total amount of solids: is estimated at.ca. 768 pounds jper day
at current operating conditions.
^ ...
Samples of solldl wastes were obtained from the
collection points in the.proposed system.. These samples weere.
representative of material!, to be obtained from the fine.powder;
sump, the wax trap the bottom of the wax separator and thee-
sump from the Dispersion Airea: The mkke-up of these saitiplees
Was as. follows * .v
-T . ''
' . . . I.,,.
.j
>.'5 :. V ,
.*. r;. L*,i*V , * ,
*
>it.'-vxu.. 'i'i''s -VV..'.\ ' OD0074~
R. F. ANDERSON
2 August 331, 196$
, t. ' *1
Fine Powder S3ump - This material looks like
contaminated,, wet, fine powder. The material
contained 36..2% water and 130 ppm perfluoro-
carbon dispersing agent calculated as C-8 'APFCC. .
1
` Wax Trap - ap>pears like wax. Lost 8* by weigiht ,
on heating to) 175C. Contains ca. 30 ppm C-8..
,
, #. ,
.*
,
Bottom of Wax: Separator - appears like wet fimev
powder and comtalns about 65* water and 240 p p m
C-8.
`
,
Dispersion Arsa Sump - This sample was actuallLy
obtained fromi the bottom of .the stabilization .
tanks and was; a mixture of-a 60* dispersion .
liquid and a isolid. containing about 30* water..
The material (contained ca. 300 ppm water. In
most of the wcork dona with this mixture, both
the liquid ancd solid phase were analysed,.
'|
i ... . ^
! V . V .`n
/; . .--Vi
;
1. Leaching
As a first step,, it was determined that the dispersing
agent could be leached frcom these solids. This was done b;y adding . .
100 grams of the sample firom tK&- different sources to 100 m l of
water in a Waring Blendor.. After blending for 5 minutes, 1the .
water was filtered and ansalysed for dispersing agent by thee
titration method (see belcow) . The data shown in Table I slhow
`'
that the C-8 dispersing agent could indeed be extracted by water/ '`7 .
ThiB is the conclusion reached by Crandell in 1964.(see atitach- ` "
ment).
Table I
^ The Extraetioon of C-8 Dispersing Agent
from "tefflon11 Samples in Water
`. ; `
Sample Source.
r-y't* . J PPM C-8 Extracted'
:
1st Extraction 2nd Extraction..
*
. -1 '*
..
.7
^`
Fine Powder Sump
'
19 *
...
>y
''
.
...
.
Wax Separator
103-; .
15,7 . *;.
Wax Trap
^
./ `SJ)
; 17
. ' .
2. Baking
` '
"*
.. ' "
' .
;
The samples wetfei baked at. 1750 for 3 5 and 20 tnours.
Analysis of these sample.s 1showed almost /complete removal off the--
dispersing agent a t o r 210'hours; after 3 hours treatment only-"
the sample from the fine powder, sump contained any residualL C-8'-" /
i -1
000075
CF020542
*4
m 3 ''
. August 31, 1966
TABLE il
ANALYSIS OP PER1PLUOROCARBON DISPERSING AGENT _________ IN "TJEPLON SOLIDS WASTE
Sample Source
Pine Powder Sump
Dottom of Wax Trap .
Wax Trap #8
Stabilization Tank Liquid Solid
. , J
Hours Heated 8 1?5C
0
.Si .
20
130. 1 100 2.7 0.*24
240
{t \V
<10
2.4
(30) j,: 0
3-
V .
460 . 0 130 <40
'X
0.73
1.1 0.20 0.77: 0.41
'/ I
1.-'. -i -.i i:V 7?" ; 'v
.
J- V '-`V V
*'*
;'i-'* -t;x ' *
'i
-.fv'..- .
,1:h *r..
: W .Vrivr
.O'
^
,!:
t . r .*
.v ., . :
;* I *>, , .
...
*
-*;
V;
' ' ". ';
` .. ') 'it *:.. ' f.`.I*..'
< .-**r' .
.
*'
. : \ .- . :
-.v
4? V - . ' .
. W- -..'Vi .>.? -MX- ./.'v.*..:* .:*: ': .*
:--- r -V ^ 'x-Xy-i
ViH -;',;.;5;V V
-..Vu*4:V ;
< ;-
-.'I. ; y/
: & '
.'W.
-7 ':
r' `k ':]
,v . ..
*1
. *;*;;iv.,'
; \ .. v
. .'< .V
.
1. #1
.t4*+ :. a v. % ...
*i
-J: 1 . i
-!{,,V*>t v>r.v;
;.'"iViV 1:T i : V../.V-C
1 iitr
T" `
--ttt*
- r * .: EID193616
000076
CF020543
R. F. ANDERSON
- k-
August 311, 1966'
APFC. The temperature of 175C was chosen as one easily reached by most ovens and because It Is below the flash point of tlhe wax used (205C).
:
3. Analysis
Two methods of analysis were used for the deternninatlon
of perfluorocarbon dispersing agents in the waste streams. The
procedures are Included heere for completeness. One made uise of
the property that perfluotrocarbon dispersing agents can bei distilled
with water from a strongljy acidified slurry. This distilliate can
then be titrated to deemmine the amount of acid (as perfliuoro-. .
octanoio acid (C7F15C20H -- MW 431). 'In these studies the following;
procedure was followed:
' 1. A 100 gram samplee (+200 nil of distilled water)'
.
was cut in a Wariing Blendor. The slurry was
added to a 500-mIL flask and 25 ml of concentrated : ' .
phosphorio acid added.
. *
2. The flask was fittted with a distilling head and condenser. The lurry was heated to boiling and the condensate collected in an Erlynmeyer flask containing 50-ml of distilled water that had been, carefully neutralized to a pink end-point with phenplphthaleln lindicator. Distillate samples ` were collected each 5 minutes and titrated with 1/100 N sodium hjydroxide. .
t .
. \
3* When the titrations indicated that no additional <acid
V
was being dlstllXLed (ca. 3 titrations or 15 minuties} ! . the tltre was addled and the amount of dispersing
agent calculated according to the following.
; , ` V
>,,, . *
. :i.A >
ppm C-- 8 ml x 43.1 .
.
This method eheckced very well with known spiked ` amounts of C-8 i m the slurry.
y
The other methodl is based on the formation of a (complex between methylene blue andl the dispersing agent. While metthylene... blue is riot extracted, fronm acid solution into chloroform, tthe complex is partitioned lntto the chloroform layer. The intensity of the coloration in the chloroform layer is related $0 thee
concentration of dispersing agent in the aqueous phase. Nconlonlo . dispersing agents, such as- "Tritoni" X-100, do not interferes The method is sensitive too 0.05 ppm dispersing agent in thee aqueous ` phase.
1 In this method, the following procedure was used;: \
it.*
1. The sample was prepared (as in the method above} \ v '
by cutting a 100 gram sample in. a Waring filendor,
I
000077
-EID193617' CF020544
J1 R. F. ANDERSON t
.v
* **
5 - August 331* 1966 .
with water, acidifying with HjPOtj and distilling.. !. For this test, 5<0-ml of distillate was collected..
2. A measured porti<on of the distillate was added to> :
a 100 ml volumetiric flask and diluted with water..
.\
The measured amoiunt depended on the-amount of C-83 "!-,V . V '
in the distillate. .For instance, in the baked
`'v '
samples, a 25 ml portion, diluted to 100 ml, was
v'
used; for the as-- received sample from the stabiliL--.
.. .'y-
zation tank, a 0..2 ml sample, diluted to 100-ral
was used.
'V
?
3 The 100-ml from 1the dilution of step 2 was added
to a 250-ml separating -funnel and 1.0 ml- of 1-9 ' /
-
HC1 solution,. 1.(0 ml of methylene blue solution
. . !/,.
(0.500 gms/liter;), and 10.0 ml of chloroform were*
added. The mixture was shaken vigorously for 2
minutes, allowed to settle and the chloroform layrerf ; '
withdrawn. .
'"
4. The chloroform ltayer was analysed in a spectro photometer in a :i-cm glass cell by scanning from ' 700 my to 600 my using chloroform in the referencia'' ' cell. The peak absorbance for the sample at 650 my was measured.
;:v
5. For these studieis, it had been.shown that 0.0057
units on the specctrophotometer 1x10"5 grams of
. * '
C-8. From the amount, of Absorbance and the factor ;V\.
from step 2, the amount of C-8 in the sample was . ^ 'v. .< *..
'calculated.
<.>>
The two methods checked, within .10% for the wax
separator sample.
....
<100078
-k. L-- -EID193618 CF020545
