*V£ «» A
*$*
-------
Table 3. Soilwasher Stuoy 9713.
Sample
No.
367-54-1
367-54-2
367-54-3
367-54-4
367-48-0
367-48-1
367-48-2
367-75-1
367-75-2
1 367-58-1
2, 367-58-2
"3 367-96-1
A 367-96-2
•3 367-96-3
^ 367-96-4
3 367-96-5
2L. 367-96-6
J 367-98-1
^ 367-98-2
1 367-85-1
•0 367-85-2
l< 367-93-1
It. 367-93-2
'I 367-97-1
»u 367-97-2
11 367-97-3
H- 367-97-4
M 367-99-1
,V- 367-99-2
Solvent
System
Toluene
Toluene
Toluene
Toluene
Toluene
Toluene
Toluene
Toluene
Toluene
Tol/lPA
4:1 v/v
To V/ 1 PA
4:1 v/v
Tol/lPA
4.1 v/v
Tol/IPA
4:1 v/v
Tol/lPA
4:1 v/v
Diesel /H-0
1:4 v/v '
Ker/H20
1:4 v/v
Ker/HoO
1:4 v/v
Ker/HoO
1:4 v/v
Ker/HzO
1:4 v/v
Extract* Sample 13Ci? TCOO
No. wt (g) Added (nq)
5
5
5
5
5
5
5
5
S
1
1
1
1
2
2
3
3
5
5
1
1
1
1
2
a
3
3
5
5
1.984
2.010
1.947
1.961
10.16
10.18
10.0
10.5
1.9924
1.9917
8.33
8.33
8.33
8.33
8.33
8.33
8.33
8.33
10.0
10.0
10.0
10.0
10.0
10.0
10.0
10.0
10.0
10.0
100
100
100
100
50
50
50
100
100
100
100
50
SO
50
50
50
50
50
SO
SO
SO
SO
50
50
SO
50
SO
50
SO
13Ci2 TCOO
Recovered (nq)
71.7
45.5
54.4
84.9
38.5
37.0
36.3
69.3
72.1
77.7
84.7
38.1
35.0
35.8
35.0
33.8
37.6
41.1
35.9
7.83
5.08
23.9
6.7
12.3
18.6
14.5
25.0
18.2
NA
X13Ci2 TCDD
Recovered
71.7
45.5
54.4
84.9
77
74.0
72.7
69.3
72.1
77.7
84.7
76.2
70.0
71.6
70.0
67.6
75.2
82.2
71.8
15.7
10.2
47.8
13.4
24.6
37.2
28.9
50.0
36.4
NA
03 Shaker Extraction Data
Native TCDD Native TCDD XNatlve TCDOb
Recovered (ug) Recovered Corrected fua) Recovered From Soil
0.937
0.634
0.695
1.124
NO
NO
NO
0.677
0.718
0.884
1.008
3.233
3.056
0.436
0.430
0.0597
0.0654
0.57
0.491
0.680
0.410
1.698
0.4143
0.235
0.229
0.102
0.147
0.524
NA
1.306
1.394
1.276
1.324
0.977
0.996
1.137
1.190
4.243
4.366
0.609
0.614
0.0883
0.0870
0.693
0.684
4.33
4.03
3.55
3.092
0.954
0.616
0.356
0.294
1.44
NA
**
85.0
89! 0
75 9X
78.' IX
10 9X
11. OX
1.6X
1.6X
12.41
13.31
64.5
60.0
52.9
46.1
14.2
9.2
5.3
4.4
21.5
NA
Extract 1 « Solvent Extract 2 « Solvent Extract 3 - Solvent Extract 4
bbased on starting concentration of 0.671|ig 2,3.7,8-TCOD/grara soil. .
NA - Not analyzed (Sample not available for analysis).
NO - Not detected.
•• - Used to establish startlnq concentration.
Water Wash Extract 5 - Soxhlet of Residue
-------
Table 3. u~«itinued)
Sample
No.
Ij 367-60-1
i^ 367-60-2
^ 367-65-3
'k> 367-65-4
if 367-78-1
It 367-78-2
*- 367-67-3
//• :;7-67-4
'^367-70-3
'« 367-70-4
- 367-72-3
l» 367-72-4
£ 367-74-3
367-74-4
'7 367-44-1
2-o 367-44-2
^ 367-65-1
^4-367-65-2
11 367-44-3
-U> 367-44-4
^ 367-67-1
1*1, 367-67-2
1 367-62-1
^ 367-62-2
U 367-72-1
2,1*367-72-2
^ 367-74-1
^l, 367-74-2
Solvent
System
II20
IX/|»d
IX/IX
IX/IX
IX/IX
IX/IX
IX/IX
IX/IX
IX/IX
IX/IX
IX/IX
IX/IX
IX/IX
2X/2XC
2X/2X
2X/2X
2X/2X
2X/2X
2X/2X
2X/2X
2X/2X
2X/2X
2X/2X
2X/2X
21/21
2X/2X
2X/2X
2X/2X
2X/2X
2X/2X
2X/2X
Extract
No.
2
2
3
3
4
4
5
5
1
1
1
1
2
2
2
2
3
3
3
3
4
4
4
4
5
5
3 Sample '
wt (g) t
9.92
9.91
8.91
10.77
3.8
3.8
8.91
10.77
8.91
10.77
8.91
10.77
8.91
10.77
9.22
9.14
8.98
9.55
9.22
9.14
8.98
9.55
9.22
9.14
8.98
9.55
9.22
9.14
8.98
9.55
8.98
9.55
3Ci? TCOO
idded (nq)
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
50
13Ci2 TCOD %
Recovered (ng)
45.3
44.4
28.0
30.0
14.0
17.2
41.2
39.4
26 (15.6)*
26.1
29.3
29.0
25.7
34.9
13.1
46.0
43.2
38.0
41.0
50.6
37.2
41.8
36.0
31.0
38.7
38.9
36.1
40.8
46.8
36.3
27.2
30.7
C]2 TCDD
lecovered
90.6
88.8
56.0
60.0
28.0
34.4
82.3
78.8
52
52.2
58.6
58.0
51.4
69.8
26.2
92.0
86.4
1 76
82.0
101
74.4
83.6
72
62
77.4
77.8
72.2
81.6
93.6
72.6
54.4
61.4
Native TCDD
Recovered fug)
0.0033
0.0036
1.51
0.799
0.231
0.307
1.26
1.39
0.812
0.682
0.067
0.097
0.848
1.353
0.982
2.89
2.87
2.63
1.03
1.21
1.12
1.10
0.218
0.288
0.325
0.263
0.12K
0.135
0.101
0.0823
0.724
0.791
Native TCOO
Recovered Corrected (uQ
0.003f
0.0040
2.70
1.33
0.825
0.892
1.53
1.76
1.56
1.31
0.114
0.167
1.65
1.94
3.75
3.14
3.32
3.46
1.25
1.20
1.51
1.31
0.30
0.46
0.420
0.338
0.173
0.164
0.108
0.113
1.33
1.29
XNative TCDnb
) Recovered From Soil
0.05
0.06
45.2
18.4
32.4
35.0
25.6
24.?
26.1
18.1
1.9
2.3
27.6
26.8
60.5
51.1
55.0
54.0
20.2
19.6
25.0
HA C
20.5
4.8
7f
.5
7.0
50
.2
2.77
2.65
1.78-
1.75
22.1
20.1
'Extract 1 • Solvent Extract 2 • Solvent Extract 3 - Solvent
bBased on storting concentration of 0.671|ig 2,3.7.8-TCDD/gra* soil.
C2l Adsce 799/2X Hyonlc NP 90.
dU Adsee 799/IX Hyonic NP 90.
Extract 4 - Hater Wash Extract 5 « Soxhlet of Residue
-------
Table 3. (Continued)
*a
iXj
?-*>
11
£
l*>
'^]
^
•Wj
/
^
f
if
5
4
Sample
No.
367-78-3
367-78-4
367-91-1
367-91-2
367-91-3
367-B4-4
367-59-3
367-59-4
367-86-1
367-86-2
367-86-3
367-86-4
367-84-5
367-84-6
367-78-5
' 367-78-6
367-88-1
367-88-2
367-88-3
367-88-4
Solvent
System
3X/3X e
3X/3X
3X/3X
3X/3X
3X/3X
3X/3X
3X/3X
3X/3X
3X/3X
3X/3X
Freon
Freon
Freon
Freon
Freon
Freon •
Freon
Freon
Freon/HeOH
4:1 v/v
Freon/HeOH
4:1 v/v
Freon/HeOH
4:1 v/v
Freon/HeOH
4:1 v/v
Extract*
No.
.1
1
2
2
3
3
4
4
5
S
1
1
2
2
3
3
5
5
1
1
2
2
3
3
S
5
Sample
wt (a)
3.8
3.8
3.85
NA
3.8
NA
3.8
NA
3.8
NA
10.0
10.0
10.0
10.0
10.0
10.0
10.0
10.0
3.8
3.8
10.0
10.0
10.0
10.0
10.0
10.0
Ci? TCDD
Added (nq)
50
50
50
NA
50
NA
50
NA
100
NA
50
50
50
SO
50
50
50
50
50
50
50
50
50
50
50
50
I3Ci2 TCOD
Recovered (nq)
18.5
20.8
16
NA
21.3
NA
14.5
NA
'59
NA
44.8
46.2
46.6
29.5
49.2
47.8
43.9
41.8
37.4
33.6
43.7
44.3
45.3
45.3
30.8
32.9
% Ci2 TCDD
Recovered
37
41.6
32
NA
42.6
NA
29.1
NA
64
. NA
89.7
92.3
93.2
59.0
98.3
96.6
87.9
83.6
74. B
87. 2
07.4
88.6
90.6
90.5
61.6
65.8
Native TCDD
Recovered (i»q)
0.54
0.604
0.167
NA
0.063
NA
0.0091
NA
0.199
NA
4.60
4.72
0.897
0.479
0.272
0.264
0.432
0.426
1.46
1.39
0.766
0.800
0.089
0.093
0.124
0.125
Native TCDD
Recovered Corrected (vq]
1.46
1.452
0.522
NA
0.148
NA
0.0313
NA
0.338
NA
5.13
5.11
0.962
0.811
0.277
0.276
0.491
0.510
1.95
2.07
0.876
0.903
0.098
0.103
0.201
0.190
XNatlve TCDDb
Recovered From Soil
57.3
57.0
20.5
NA
5.8
NA
1.2
NA
13.2
NA
76.6
76.2
14.3
12.1
4.09
4. OB
7.3
7.6
76.5
B1.2
13.0
13.4
1.45
1.51
3.0
2.8
C3I Adsee 799/3Z llyonlc NP 90.
-------
Table 4. Effect of Surfactant Concentration on TCDD Recovery
Starting Concentration 671 ng/g on Soil
% TCDD Recovered
Surfactant
Concentration
1% + JXa
2% + 2%
3% + 3%
Stage
1
32. 8b
55.2
57.2
Stage
2
25.0
21.3
20.5
Stage
3
22.1
6.1
5.8
Stage
4
2.1
2.2
1.2
Nominal
Residue
Concentration
(ng/g)
121
102
103
% TCDD
Recovered
Stage
5
27.2
21.1
13.2
True
Residue
Concentration
( ng/g )
182
142
89
Total
X TCDD
Recovered
109.1
106
97.9
a% - Adsee 799 + Hyonlc NP 90 1n Delonlzed water.
All recoveries based on average of available data points.
-------
11mlt for those experiments was 0.2 ppb TCOO on the soil. This table also
Includes a glassware system blank.
The data in Table 6 show that when 1024 yg of native TCDO was spiked on virgin
soil and the soil was extracted by the Soxhlet procedure, an average of
986.5 ug of native TCOO was recovered or a 96.3% recovery of the spike after
correction for 13Ci2 recovery.
D141-EA-4
-------
Table 6. Soxhlet Virgin Soil Spikes
Sample
1
2,
13C12TCDD
Added (nq)
100
100
Native TCDO
Added (nq)
1024
1024
C12TCOO Native TCDD
% Recovered Recovered (nq)
69.3 977
72.1 996
Average 986.5
-------
Soxhlet Extraction Procedure
1. The Soxhlet apparatus containing a clean glass thimble must be thoroughly
rinsed with solvent before using. It must be operated for 2 hours with toluene
prior to use.
2. Transfer a 10-g aliquot of a1r-dr1ed soil directly Into a suitable glass
container such as a beaker or flask.
3. Add 50 uL of a 1.00 ng/uL solution of 13Ci£ Isotoplcally labeled
2,3,7-8-TCDO directly to the soil.
4. If the soil has not been a1r-dr1ed, add 20 g of sol vent-extracted anhydrous
sodium sulfate and mix thoroughly using a stainless steel spoon or spatula.
(Extremely wet samples may require prior centrlfugatlon to remove excess water.)
Allow the mixture to stand under ambient conditions. Mix again after 2 hours
and allow to stand for at least 6 additional hours. Mix again just before
adding solvent.
5. Add 10 g of anhydrous sodium sulfate to the thimble. Transfer the sample
(soil plus sodium sulfate) to the thimble and cover with a layer of clean glass
wool. Rinse the container with toluene and transfer to the apparatus.
6. Introduce 130 wL of pesticide grade toluene Into the extractor and operate
the apparatus for a minimum of 25 cycles (18 to 24 hours).
7. The toluene extract Is transferred to a 500-mL round bottom flask followed
by two 20-mL toluene rinses. Toluene 1s removed by attaching a snyder column to
the round bottom flask and heating with a heating mantle. Concentrate to
approximately 10 ml. Then quantitatively transfer the toluene to a 20 ml vial
using 3 X 3 mL MEClg rinses. Evaporation of toluene 1s continued using filtered
N2 gas. When the volume 1s reduced to about 200 to 300 uL, an aliquot of 1 ml
of hexane 1s added to the 20 ml vial. Reduce the volume to 200 to 300 wL with
N? gas. Repeat the addition of 1 mL of hexane and again reduce to 200 to
300 uL. This concentrated hexane extract 1s ready for cleanup according to the
procedures 1n the following section.
-------
TCOO Sample Clean-up Procedure
Option A
1. Pack a 1 X 10 cm chromatography column with 1.0 g of silica gel* and 4.0 g
of 40% w/w sulfurlc acid-modified silica gel. Pack a second chromatography
column (1 X 30 cm) with 6.0 g of alumina* and a 1-cm layer of sodium sulfate.
Add hexane to the columns until free of channels or air bubbles. This can be
readily achieved using a small positive pressure (5 ps1) of clean nitrogen.
*S1l1ca gel (for column chromatography. type 60, EM Reagent, 100 to 200 mesh) and
alumina (add alumina, AG 4, BIO-RAD Laboratories) are Soxhlet-extracted with
CH2C1? for 21 hours and activated at 130°C and 190°C, respectively, before use.
Each Batch should be tested for proper recovery of 2,3,7,8-TCDO before use.
2. Place the hexane extract on top of the silica gel and rinse the culture tube
with 2 X 0.5 ml of hexane onto the column and elute directly onto the alumina
column with 45 ml of hexane. Discard the silica gel.
3. Place 20 ml of hexane on the alumina column and elute until the liquid has
dropped below the sodium sulfate layer. Discard the eluted hexane.
4. Place 20 ml of 20% v/v methylene chlorlde/hexane solution on top of the
aluminum. Collect this fraction 1n a 125 ml Erlenmeyer flask.
5. The volume of this eluate which contains TCDD 1s reduced by a gentle stream
of filtered nitrogen gas. When the volume 1s down to about 1 to 2 ml, allquots
are transferred, one at a time, to a 2-mL conical m1n1-v1al for further concen-
tration until the entire fraction 1s transferred. One ml of hexane 1s used to
r1<«e the Erlenmeyer flask and 1s transferred, 1n portions, to the m1n1-v1al.
Repeat this procedure once more. At no time must the extract be allowed to go
to dryness. Finally 500 uL of hexane 1s used to rinse the walls of the mlnl-
vlal. The sample 1s stored at this point 1n a freezer until analysis. Just
before analysis begins, the hexane volume 1s reduced to almost dryness and
Isooctane (or other Cg to CH hydrocarbon) 1s added to obtain a final volume of
50 uL. This final addition of Isooctane includes the Internal standard
37Cl4-2,3,7,8-TCDD.
Option B
1. Prepare a glass macro-column, 20 mm 00 X 230 mm 1n length, tapered to 9 mm
00 on one end. Pack the column with a plug of sllanlzed glass wool, followed
successively by 1.0 g silica gel, 2.0 g silica gel containing 33% (w/w) IN NaOH,
1.0 g silica gel, 4.0 g silica gel containing 44% (w/w) concentrated H2S04 and
2.0 g silica gel. Add hexane to the columns until free of channels or air
bubbles. Quantitatively transfer the concentrated sample extract to the column
and elute with 90 ml hexane. Collect the entire eluate and concentrate to a
volume of <1 ml 1n a centrifuge tube.
2. Construct a chromatography column by packing a 5 ml disposable plpet (cut
off at the 2.0 ml mark) with a plug of sllanlzed glass wool and add 1 g or
activated Woelm basic alumina (activated at 600° for 24 hours) to the tube.
-------
TCDD Sample Clean-up Procedures (Continued)
3. Quantitatively transfer the concentrated extract from Step 1 to the top of
the column using 2 ml hexane.
4. Elute the column with 5 ml of 3% methyl ene chlo£1de-1n-hexane and discard
the eluate.
r;
5. Elute the column with 20 ml of 50% methylene cflor1de-1n-hexane and retain
the entire column eluate for analysis. - ^ «„
i ^1- -T
6. Concentrate the eluate to a volume <1 ml and quantitatively transfer 1t to a
2 ml conical ra1n1-v1al.
7. Further concentrate the extract In the m1n1-v1al t* near dry ness, and store
the extract at 5°C until $ist before GC/MS analysis. . ^ "
~-3F~
8. Prior to GC/MS analysis, reconstitute the extract by adding Isooctane (or
other Co to Ci4 hydrocarbon) and adjusting the final volume to 50 uL. This
final add1t1ofcof Isooctane Includes the internal standard 37Cl4-2,3,7.8-TCOO.
____ ~Tf <£. -.,,.
Option C
Certaln very dirty samples may require preliminary, cleanup before column
chronatography. For those situations, the following-procedure 1s suggested:
~~ _ * -3&
1. Wash the organ1% extract with 30 ml of 20% aqueous jK>tass1unrt>ydrox1de by
shaking Tor 10 minutes and then remove, and disetrd the"$qt»eous layer. -
2. "iasfc the organic extract with 25 ml of doubly distilled water by shaking for
2 mlnutH and again remove and discard the aqueous layer.
-^
3. CAUTIOUSLY add 50 ml concentrated sulfuMc acid to the organic extract and
shake ror lu minutes. Allow the mixture to stand until the aqueous and ouanlc
layers separate (approximately 10 minutes) and remove and discard* the aqufwjs
acw layer. Repeat add washing until no color is visible In U£ add layer.
-T IT
4. Add 25 ml of doubly distilled water to tht organtc extract and shake for
2 minutes, remove and discard the aqueous layer and dry th«-organic lajftr by
adding 10 g of anhydrous sodium sulfate.
5. Transfer the organic extract to a centrifuge tube and concetiPite to near
dryness by placing the tube In a water bath: at 55°C, wh1le*f>ass1ng a gentle
stream of filtered, prepuMfled N2 over the surface of the extract.
Reconstitute 1n hexane before proceeding with the column chromatography
(Option A or B). .,=
D141-EA-AP-6 *
-------
APPENDIX B
-------
TCDD INSTRUMENT PROCEDURE
INTRODUCTION
This 1s a qualitative and quantitative (high resolution) GC/(1ow resolution) MS
analysis specific for tetrachlorod1benzo-p-d1ox1n using selected 1on monitoring.
The soil sample extract 1s spiked with I3c12 2,3,7,8-TCDD before concentration
and cleanup. The recovery of this Isotoplcally labeled compound corrects for
the cleanup procedure and concentration steps. The final concentrate containing
the native and Isotoplcally labeled TCDD Is taken to near dryness and brought
back to a known volume with an Isooctane solution containing a known con-
centration of 37Cl4.2,3,7.8-TCDD. This Isotoplcally labeled compound acts as
an analytical Instrument Internal standard to correct for small variations 1n
Injections and Instrument performance. Quant1tat1on 1s based on the response of
the native and "C^ labeled TCDO relative to 37CU-TCDO as the Internal stan-
dard. Nominal detection limit 1s 1 part per billion based on the original
sampl e.
SAFETY
Samples generated during the experiments are handled by qualified personnel
only. The experimenter and the analyst must be adept at safety procedures and
have a working knowledge of safety protocols. GC/MS Instruments used for dloxln
analysis must be equipped with vapor contamination traps on the capillary split
and sweep vents and on the roughing pumps' effluent lines before use.
INJECTION PROCEDURE - HOT NEEDLE TECHNIQUE
The syringe must be thoroughly cleaned between Injections to avoid cross con-
tamination. Remove the plunger between Injections and wipe 1t thoroughly with a
K1mw1pe. Rinse the syringe with ten to fifteen full syringe volumes of hexane
solvent wash. Replace the solvent wash with pesticide quality hexane dally. If
a Hamilton syringe cleaner Is available that Is equipped with a vacuum source,
use this also. Do not use the Hamilton syringe cleaner 1f there 1s no vacuum
pump attached. Insert the needle Into the septum port, wait approximately ten
seconds for the needle to heat, then pump the plunger back and forth a few
times. Rinse with the solvent wash hexane again. Work the plunger up and down
1n the syringe barrel to reduce excess hexane wash. There should be approxi-
mately 0.5 uL of solvent left 1n the syringe barrel following this final rinse.
Draw back the plunger so that about 2 uL of air 1s 1n the barrel. Draw 1.0 of
sample Into the needle. Usually to get a total of 2 uL of sample, 1t 1s
necessary to pull the plunger back approximately 1.2 uL. The sample should be
drawn up Into the barrel and the amount confirmed to be 2 uL. If 1t 1s not, the
sample should be expelled and the process repeated.
After getting 2.0 uL of sample Into the barrel, Insert the needle Into the
Injector port and wait 6 seconds. Rapidly make the Injection.
After making the Injection, remove the needle as quickly as possible. As soon
as the Injection 1s made, start the GC.
-------
METHOD
Setup and Installation
Step 1 Install a 60-meter, 0.25-mm ID fused silica SE54 capillary column.
Set the head pressure to approximately 15-20 ps1 and the split and
sweep flows to 30 mL/m1n and 6 mL/m1n respectively.
Step 2 Establish the appropriate MS Instrument conditions by optimizing the
sensitivity for a low TCOD standard. The optimization technique
requires sequential adjustments of the MID descriptor (Ion scanning
rate), electron multiplier voltage, and Instrument resolution based on
FC43 tune. Instrument zero should be adjusted to give a reasonable
background collection without serious loss of analytical signal.
Step 3 Set GC conditions
Injector temperature 300°C
Initial oven temperature 80°C
Initial time 2.5 mln
Secondary oven temperature 200°C
Ramp rate 1 20°C/m1n
Final oven temperature 300°C
Ramp rate 2 !OaC/m1n
Hold time at final temperature 5 mln
Separator temperature 300°C
Split/sweep time 90 sec
Filament/multiplier off time 600 sec
Filament/multiplier mode Auto
Insert mode Capillary
Manifold temperature 100°C
Step 4 Standards Calibration
A three-point Instrument calibration curve 1s created to establish
linearity of Instrument response. Standards containing 400, 1000,
5000 pg/uL of native TCDD respectively with 100 pg/uL 37Cl4-TCDO each
and 200 pg/uL 13C12-TCDO each are run under the conditions established
1n Step 2. Response factors are calculated and subsequent analyses
require only one standard (usually 5000 pg/jiL) 1f the response factors
do not change from the original calibration. Response factors are
calculated as follows:
R » Area for native TCDPa x Cone of 37Cl4-TCDD
fn " Area for 37Cl4-TCDD Cone of native TCDD
R , Area for 13Ci2-TCDD x Cone of 37Cl4-TCDD
Area for37Cl4-TCDOb Cone of l3Ci2 TCDO
-------
Step 5 Sample calculations
Native rrnn in m Area for native TCDD8 Y 1 v u~i * *. ^ • . % - -
native TCDD m » _ _ x X Vol of extract (yL) X 0.1 ng/yL
Area for 37Cl4TCDDb RfN
0.1 ng/uL - Concentration of 37Cl4-TCDD 1n sample extract (ng/yL)
TCDO 1. - *™ ;°r ,12-TCO° X -L X vol of «tnct {*) X 0.1
Area for 37Cl4-
X 13C12 TCOO recovered - "9 "C12 TCDD recovered 1n extract x 100%
ng ISC12 TCOO added to sample
Corrected native TCOO recovered - "*\\™ TcjO 1n extract (ng) x 10°
* "^12 TCDO recovered 1n extract
% native TCDO recovered In sample - Corrected native TCDO recovered (ng) X 100
Metgnt or original sample igj A starting
cone (ng/g)
Where:
a - Sum of areas for 1on 320 and 1on 322
b - Area for Ion 328 -(0.009 X area for 1on 322)
c * Sum of areas for 1on 332 and 334
Response factor for nature TCOO
Rf I » Response factor for l3Ci2-TCOO
-------
8.2 SOIL CHARACTERIZATION
Preliminary soil characterizations were completed by Raamot Associ-
ates (Raamot, 1983). Grain size analyses, determinations of natural moisture
content, and Modified Proctor compaction tests were undertaken to develop
moisture/density characteristics and determine optimum moisture content for
permeability testing at various densities. Figure 24 presents the grain size
distribution curve of the Freehold series soil as determined by Raamot.
Figure 25 presents the compaction test report showing maximum compaction of
approximately 1890 kg/m3 (118 lbs/ft3) at US moisture content. Permeability
and density data are presented in Figure 26. All of these procedures were
completed using ASTM methods as noted in the figures.
After these Initial tests, SAI/JRB completed additional soil
characterizations. The additional testing Included
• Grain size distributions determined by wet and dry sieve pro-
cedures and pi pet analyses;
• Percolation rates under constant head versus compaction/density
relationships as expected in the soil columns used to simulate
CAT tank testing;
• Mineraloglcal determinations by X-ray diffraction;
• Total Organic Carbon (TOC);
t Cation Exchange Capacity (CEC).
Table 36. presents the grain size distribution obtained by wet sieve
and pipet analyses. In comparison with the Raamot analyses, as the data
illustrate, significantly higher percentages of fines (15S silt and 8* clay)
were obtained using the wet sieve and pipet techniques. Approximately 95* of
the theoretical surface area 1s represented by these fine particle sizes.
This calculation assumes spherical particle shapes and 1s based on the mass
and surface area relationship of each size Interval (I.e., diameters of 4, 2,
1, 0.5, 0.25, 0.125, 0.062, 0.031, 0.016, 0.008, 0.004, 0.002 and 0.001 mm).
To determine the effect of the degree of soil compaction on the
percolation rates in the soil columns being used to simulate CAT tank
8-18
-------
U.A •TANOAIIO SIEVf NUWUR
» • » t> !•«•*•
00
I
VO
•UMIMSUII | COMLCS
CLAttiriCAliON
tMJUOl MMIIM/TKATMUT UM HUM THIM fAUI. KM JI»U»
«* r MM. tr«ci
Ht
Silt. U.c« r Orwl.
GRADATION CURVES
RAAMOT ASSOCIATES
FIGURE 24 Standard Grain Size Gradation Curve from Raamot Associates (Raamot. 198.1).
-------
00
I
M/l
|4O
t,.n
3IS°
1
E«o
||IZO
•
M
t
I
too
vu
1
1*1
\
ri
•
ec
INI
/
|
rn
,/
o
T.
^
P
x
M
Cl
>>
|
NT
6
or
0
•Y
•
2
IM
o
NT
y
.
A
COMPACTION TEST REPORT
PROJECT'
OKMCU. IMITin/tKMKNI UW
KIM INIH mil. NfM Jf«UI
SOURCE* ,,'....
curtttarf rit
TYPE FILL1
DESCRIPTION i M-|T*M c»» r MM. •
TFftT UFTMnni ASIN t-KSI. Mtfthorf C
SAMPLE NO.: |
tyfl.^M.if. 1U.I.M III
y«. D>i. OMiHi lli>e»
a^i.i.. tf^.f CMMI Cm. lit
HOT "rr «t-«"f *•" f««
RAAMOT ASSOCIATES
COMCULTINf tmiNUIIS
DATE* ftkriMry I. INI
•
FIGURE 25 Compaction Test Results from Raamot Associates (Raaraot, 1983)
-------
00
f\J
!.• i
lllllilliiiimillllllllMIIIIIIMIIIIIIIIIUIIIIIIIIIIMIIIIIIM
i!!!!:1.1.1,1,:!!1.!;::::::::!:::::::::!::::::!!!:::!::!::
iiiiiiiiii iiiiiiiimiiiiiii.:«iiiiiiiiiiiiiiiiiiiiiiiiiiiiiiiii
!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!ii!!!!!!!!!!!!!!!!!!!!!!
iiiiiiiiilllliillliiiilliliiiiiiiiiiiiliii!!!!!!!!!;!!!!!!!!!!!!!
• i i i i ii iiiiiiiiiiiiiiiniiiiiiiiiiiiiiiiiiiiiiijiiii ii ii
iiiiiiiiiiiiiiiiiiiniiiiiiiiiiiiiiiiiiiii !!!!!!!!!!!!!!!!!!!!
i ir1
IN IN l« IM IM IU III . Ill 111 ll« IK Hi IU
•>.• M.« N.I •!.« M.« M.l N.I M.I M.l M.I W.I M.I. M.I
DRY UNIT WEIGHT, IJ , (pel)
COMPACTION (P«rc«n» ModlfUd Preolor Otnilly)
PERMEABILITY VS. DENSITY
RAAMOT ASSOCIATES, RA.
8AUR.C SOURCEICimSMM Ml
PROJECT: CNHHOL
™" nwmum
I HIM fttU. KM JHSH
FIGURE ?6 Permeability Versus Density Relationship from Raamot Associates (Raamot. 1983)
-------
TABLE 36 Grain size distribution of Freehold Sill by . ^
Wet Sieve and PI pet Analyses (Modified ASTlfD-422 9
~ using U.S. Bureau of Soils Sieve sizes). ^
Class
Gravel
Sand
Silt
Clay 7
:|pkze Range
>1000ym
- 62yro to lOOOim
8un to 62yro
<8udi
Mass
(percent)
16
61
15
8
Theoretical
Surface Area^H
^C percent)
<.05 ,
5
«*
"" *? 61 ' "^ ,
8-22
-------
performance, the soil was packed (as received) with a natural moisture content
of 10 to 12%. Using a percent moisture content of 115 and compacting the soil
1n the columns to a density of 1680 kg/m3 (105 Ibs/ft3), an optimum percola-
tion rate of 1.5 x 10"3 cm/sec (4.9 x 10"5ft/sec) (I.e., discharge rate
divided by column diameter) was obtained under a constant 60 on head (24 in).
The soil column experiments and percolation rate measurements were undertaken
to provide an estimate of the expected aqueous surfactant flow under field
conditions.
To determine the mineralogical composition of the Freehold soil,
X-ray diffraction"studies were undertaken by Technology of Materials Company,
Santa Barbara, California. The sample was prepared by grinding and sieving an
aliquot of soil to 200 mesh particle size. This powder was then run 1n a
Phillips Electronics X-ray d1ffractometer, equipped with a crystal monochro-
meter. The X-ray diffraction charts were analyzed and phase Identifications
were made by comparison with standard data in MCPDS/ASTM diffraction files.
(The report 1s presented in Appendix F.) The results showed quartz and
feldspar to be the only measurable constituents. Quartz was the major phase,
representing at least 98% of the total weight. Measurable amounts of any clay
minerals did not appear in the native sample or 1n an additional sample
prepared using a separation of the clay s'lzed particles by suspension in
water. The color of the Freehold soil suggested iron carbonate or a hydrated
iron oxide; however, this color is evidently caused by an Morpheus iron oxy*
hydroxide or hydroxide, because measurable peaks were not found representing
the suspect phases.
The total organic carbon content (TOC) of the soil, as measured by
Laucks Testing Laboratories, Inc. (using a Dohrraann DC 80 TOC Analyzer), was
determined on a sample of soil prepared by grinding and suspending 1n an
aqueous solution of phophorlc add and sodium phosphate, in accordance with
EPA Method 415.1. Th* TOC valirt MS O.IK by Might, This relatively low
level of organic matter In the soil Implies a relatively low contribution by
organic matter to the adsorption potential for organic contaminants.
The cation exchange capacity (CEC) of the soil was also determined by
Laucks Laboratories. The soil was dried and sieved through an 18 mesh screen
S-23
-------
and the CEC was determined by the methods of Jackson (1960). The totarl
exchangeable metallic cations and the exchangeable hydrogen were determined,
and the results were combined to yield the total CEC. 3w result was 8.6 •
aiUiequiv«l«*ts ?«r 101) gnu,*an extremely low value, confirming the absence »
of wlneralogls «Uy 1n the soil jt The reports of the soil characterizations
performed by Laucks Laboratories are presented 1n Appendices G and H.
-------
APPENDIX G
TOC ANALYSIS
-tfing Laboratories, Inc
jcuih Hamey 5m«.5e«it>J*ahin?lcn 98X38 '206)757-5:60
Certificate
andlechrucalGa VJUM
Associates
476 Prospect- St.
La Jolla, CA 9-2038
ATTN: Daniel Jf. Baxter
SOIL
80702
April 22, 1!
P-0- 288677
Marked: Clarksburg Sediment
Total Organic Carbon, %
— 0.12
Respectfully submitted,
» • *
Laucks Testing Laboratories, I:
JMO: vb
I ««•>*•» MM 01 I
-------
'L
, *sting Laboratories, Inc
APPENDIX H
CEC ANALYSIS
Certificate
juih Hamey 5iM«t. Seattle Ufcshinqjon 98108 (206) 767-5060
." misryMkJofcacio^y and Technical Ss vk.es
Science Applications, Inc.
1200 Prospect St.
P. 0. Box 2351
La Jolla, CA 92038
HTQN
SOIL
30971
May 31. 1332
P0= 365203
» "U
C
Marked: Clarksburg Soil
Dried and sieved through an 18 mesh screen
'I PffMFQftMCD
« SSULTS.
Cation Exchange Capacity • 8.6 meq Na/100 grains
Respectfully submitted,
Laucks Testing/Laboratories, Inc.
Mike Nelson
MN:bg
«•• e« iix utne*. nni*mt*. m i«n«r«i««
•TMM«««nT
M *««MI«<• I
-------
; Adsee 799
Spreader-Penetrant
Organics Division, Witco Chemical Corporation
Bulletin 255 September 1981
Adsee 799 surfactant is a multipurpose spray tank additive developed for use as a penetration aid and
wetting agent. One of the major uses of Adsee 799 surfactant is as a penetration aid for
"hydrophobia" or hard-to-wet soils. The addition of this surfactant to aqueous systems increases the
rate at which water is able to penetrate these soils.
Penetration modifiers offer the advantages of decreased soil erosion, unproved water drainage,
decreased water runoff and increased utilization of soil moisture by plants during hot weather condi-
tions. Other potential areas of research include its use as a soil conditioner for plants and trees and as.
a germination aid for seeds and bulbs.
Typical Properties
Appearance Slightly hazy liquid
pH,5%in 1:3isbpropanol/water 5-7
PourPoint,°C(°F) 0 (38)
FlashPoint, PMCC, °F >200
Specific Gravity at 25/4eC(77/39°F) 1.04
Suggested Use Rates
Per 100 Gallons of Water
General Soil Conditioner 1 -2 pints (per 1000 sq.ft.)
Penetration Aid for Irrigation 2-4 pints
Preplant Conditioner for Trees and Shrubs 4-6 pints
Storage
This product should be stored in tightly closed containers in a cool, dry area.
Witco
-------
Ptocaaa ovamtcaia Ptvtxon
'Diamond Shamrock Cotputafaon
350MtKembteAv«nue
Mocrtstown. New Jersey 07960
Diamond Shamrock
Hyonic' NP Series
Product Bulletin
OEN-tt
The Hyonic NP Series of nonionic surfactants
are potyethoxytated nonylphenols with
average ethylene oxide contents off-12 moles
per mole of nonylphenol. Each surfactant
provides a unique combination of detergent,
emulsifying and wetting properties which
depend on the amount of ethylene oxide on the
lipophilic portion of the molecule.
The Process Chemicals Division currently
offers six Hyonic NP nonionic surfactants
which can be used alone or with other
surfactants for a variety of uses involving
detergency and wetting problems.
This brochure is designed to assist in selecting
the Hyonic NP surfactant best suited to each
application.
Typical Properties
Product
Appearance
Moles E.O.
HLB
Activity. %
Density, Ib/gal
g/ml
Solubility, aqueous
Cloud point. «F/»C
(1% aqueou* solution)
Pour point. *F/°C
pH. 1% aqueous solution
Hyonic
NP-40
Clear
Liquid
4
9
>99
8.5
1.02
Dispersible
127/53
-21/-29
7.0
Hyonic
NP-60
Clear
Liquid
6
12
>99
8.7
1.04
Dispersible
127/53
-18/-28
7.0
Hyonie
NP-90
Clear
Liquid
9
13
>99
8.8
1.06
Clear
Solutions
129/54
36/2
7.0
Hyonie
NP-100
Clear
Liquid
10=
132
>99
8.9
1.07
Clear
Solutions
154/68
40/4
7.0
limniln
nyonic
NP-110
Clear
Liquid
11
13.6
>99
8.9
1.07
dear
Solutions
162/72
55/13
7.0
Hyonie
NP-120
Liquid to
semisolid;
Clear liquid
melt
12
14
>99
8.9
1.07
Clear
Solutions
196/91
59/15
7.0
10 «copBonoicona»oniore»e>»nBinroi
NOTMt
noy ov nocMUOf
rge
•*
Prirftad in U.S.A.
•Diamond Shamrock Corporation 1983
-------
Product Bulletin
Surface Active Properties
Product
Surface Tension
Dynes/cm 0.01%
solution at 77*F/25°C
Wetting Test (Draves)
3 g hook, % required
for a 25 second test
Ross Miles foam Test
77°F, 0.05% solution
in distilled water
mm Initial Foam
mm foam after 5 min
Applications
Hyonlc
NP-40
28
Insoluble
Insoluble
Insoluble
Hyonlc
NP-M
30
0.21
10
7
Hyonlc Hyonlc Hyonlc
NP-90 NP-100 NP-110
Hyonlc NP-40
Hyonlc NP-40 surfactant is a nonionic
emulsifier useful in many formulated products.
Among its applications are. the following:
Emulsifier for solvent cleaning compounds
Emulsifier for "waterless- hand cleaners
Low foaming emulsifier for silicone
products
Solvent based metal cleaners
Detergent for petroleum oils
Viscosity reducer for plastisols
Intermediate for production of anionic
surfactants
Emulsifier in agricultural emulsifiable
concentrate formulations
Hyonic NP-60
Hyonic NP-60 is a multi-purpose nonionic
surfactant which has found application in the
following areas:
• Emulsifier for textile lubricants
• Wetting agent for textile fibers
• Intermediate for textile antistats
• Detergent for all phases of textile
processing
• Color development enhancement in latex
paint
• Polymerization post - add stabilizer
• Emulsifier in agricultural emulsifiable
concentrate formulations
• Color acceptance agent for tinted coatings
31
0.04
52
47
32
0.05
90
80
34
0.07
105
95
Hyonlc
NP-120
36
0.12
115
105
• Eliminates color-pull in tinted coatings that
results from defoamer use
• Helps eliminate "fish eyes" and other
wetting problems in coatings caused by
excess defoamer
Hyonlc NP-90
Hyonic NP-90 has many uses involving
detergency and wetting problems. It will
continue to perform satisfactorily even if its
cloud point is slightly exceeded. Hyonic NP-90
has found favor as a co-emulsifier. It may be
used as follows:
Detergent for household and industrial
cleaning compounds
Detergent-penetrant for acid cleaning
solutions
Alkaline salt cleaners
Degreasing compounds
Detergent for all phases of textile
processing
Wetting agent for paper towelling or tissue
Paper deinking
Emulsifier and wetting agent in agricultural
applications
Hyonlc NP-100 and Hyonlc NP-110
Hyonic NP-100 and Hyonlc NP-110 are
versatile surfactants which strike the optimum
balance between solubility and detergent
properties. Their range of application is
broader than other members of the series and
includes:
-------
Product Bulletin
'' » Bases for liquid dishwashing detergents
• Detergents for low temperature laundry
preparations
• Wetting agents in mineral acid and alkali
solutions
• Bases for household and industrial
formulated cleaners
» Penetrants for corrosion inhibitors
> Emulsifier adjuvants in liquid formulations
• Stabilizers for latex preparations
• Rewetting agents for paper, towelling and
tissue
> Hide soaking
• Paper deinking
• Emulsifiers and wetting agents in
agricultural applications
Hyonte NP-120
tyonic NP-120 consists of approximately 12
.notes of ethylene oxide per mole of nonyl
phenol. This ratio permits excellent detergency
nd wettability for
* High temperature detergent formulations
* Detergent-penetrant use in concentrated
,, olutions of electrolytes
Vetting agents in caustic solutions
* Coemuisifiers for oiMn-water emulsions
DA and EPA Status
Food Packaging Use
he Hyonte NP series of nonionic surfactants
Jiscussed in this brochure comply with the
following indirect food-contact applications of
I CFR:
175.105 Adhesives
176.180 Components of Paper and
Paperboard in Contact with Dry
Food
176.210 Defoaming Agentt Used in the
Manufacture of Paper and
Paperboard
.78.3120 Animal Glue
178.3400 Emulsifiers and/or Surface-Active
Agents
Agricultural Use
Hyonte NP emulsifiers are cleared by the EPA
under 40 CFR. 180.1001 (c) and (e). Paragraph
(c) of this regulation exempts residues from the
requirement of a tolerance when used in
accordance with good agricultural practice as
inert (or occasionally active) Ingredients in
pesticide formulations applied to growing
crops or raw agricultural commodities after
harvest Furthermore, clearance, under this
section enables a grower or applicator (by
reference to 21 CFR 182.99) to add these
surfactants to a pesticide use dilution prior to
applying it to a raw agricultural commodity.
In addition, these nonionic surfactants also
comply with FDA regulation 21 CFR 172.710
which permits a grower or applicator to add
them to a pesticide use dilution before
application to a growing crop.
All Hyonte NP emulsifiers comply with
180.1001 (e). a list of exempt inert ingredients
which can be used in pesticide formulations
applied to animals. They should be evaluated in
your toxicant formulations for this application.
Packaging, Storage and Handling
Hyonte NP surfactants are shipped in 55 gallon
(200 liter) steel drums and bulk. No special
handling or storage precautions are necessary.
Additional handling information is contained in
material safety data sheets which are available
on request
Freight Classification
Members of the Hyonte NP series are classified
as: Cleaning, Scouring or Washing
Compounds NOI; or Soap, NOI Liquid or other
than Liquid or Soap Powders.
QEN-M
2/83
-------
Product Bulletin
-------
SOLVENT
DATA
BULLETIN NO. FST-1
"FREON" TF SOLVENT
INTRODUCTION
"Freon" TF is trichlorotrifluoroftharm, a member of the
family of fiuorocarbon chemicals developed and marketed
under Ou Font's trademark, "Freon". Originally developed
as refrigerants, these compounds are now widely used as
solvents and cleaning agents, fire extinguishing agents, di-
electric fluids, aerosol propeUants, chemiral reaction media
and coolants. In common with other memben of the flooro-
-arbon family, "Fieon" TF is nonflammable, chemically and
jermally stable, low in toxicity and recoverable by distilla-
flbn without decomposition.
This same chemical is also marketed as "Preon" Precision
OgMimj Agent under a different product' specification that
controls particulates and sets a slightly higher standard for
nonvolatile matter.
The applicable military specification for trichlorouifluoro-
ethane is Mil-OS 1302B (Type I applies to "Freon" PCA
and Type II applies to "Freon" TF).
sensitive parts from damage. This property also helps
to bold soils in the boiling solvent and prevent distil-
lation into the vapor zone where they may be re-
deposited on objects being given a final vapor rinse.
Since the chemistry of soils varies greatly, the chemistry
of the cleaning agent must be similarly adjusted to remove
them. For this reason, "Freon" TF is also used as the base
for a variety of "Freon" solvent formulations, all of which in-
herit desirabk properties of their parent and extend the
cleaning action of "Freon" deaning systems to cover a
significant range of the spectrum of soils. This bulletin
describes only the properties and uses of "Freon" TF;
bulletins giving similar information for "Freon" solvent
formulations can be obtained by calling one of the phone
numbers on the last page or from an authorized "Freon"
solvent distributor.
"FREON" TF AS A CLEANING SOLVENT
"Freon" TF is useful not only because of the properties
enumerated above but
1. It has a very low surface tension, enabling it to wet
surfaces and get between soils and the surfaces on
which they are deposited, thus assisting hi removal of
the soil
2. It has a high density, which helps to displace soils
from surfaces of parts being cleaned and to float
these soils to the surface of the solvent.
3. It has an unusually low latent beat of vaporization,
which means that the condensing vapor necessary
in vapor degreasing processes can be generated with
low energy input
4. It has a low boiling point (117.6T at sea level) so
parts being cleaned in boiling solvent are cool enough
to handle immediately while protecting temperature-
TaMe of Contents Page
Introduction 1
"Freon" TF as a Cleaning Solvent 1
Physical Properties 2
56MCDM SOfWfn PDWGT 2
Effect on Materials of Construction 3
Electrical Properties 7
Penetration and Wetting Power 7
Surface Tension 8
Stability 8
Purity 9
Cleaning Processes, Equipment and Uses 9
Applications 9
Safety 10
Environmental and Occupational Legislation 11
Specifications 11
Packaging and Availability 11
•FREON is Ou Font's r«cist«r««l tr»d«m»rk tor its Huorocartton compounds.
-------
PHYSICAL PROPERTIES
"Freon" TF is a pure, stable, chemical compound. It is a
clear, dense, colorless liquid having a faint solvent odor.
Table I lists the physical properties which characterize
"Freon" TF. Liquid density and vapor pressure curves of
"Freon" TF as a functioa of temperature are given-in Figures
land!
FIGURE 1 liquid Density vs. TempertriureT?
Table I. Physical Properties
of "FREON" TF
Chemical Formula
Molecular Weght
Boiioi Point at OM Atmosphere, f
•C
Fraeanf Point, f
•C
Critical Temperature, *F
•C
Critical Pressure, psii
atm
Density at 77*F(2S*C)
Liquid. fes/fiL
Ibs/m
CCItF-CClFi
187.4
117.6
47.6
-31
-35
417.4
214.1
495.0
317
13*
S2.C9
Saf d Vapor at boiinf point. lbs/R>
grams/Stw
Lstmt Hist of Vaporization at b.p, Btu/Ib
csl/|nm
Spacific Heat at TtTF (2L1*C). Bht/Ob) CO or csl/f ran CQ
'Liqaid
Saf d Vapor (Cp)
Thermal Conductivity at
Uqyid
SaTd Vapor
Vlseoaty at TVf (21.1'C). Cenbpaists
Uqoid
SaTd Vapor
Rtfradh* Index of IJqwd at Mff (21SX)
Sarfact Tenson at 77T (ZS^ftM/oi
Rtlalno Oieioctrie StraMfOi (sfTnis*- 0
Li««d it 77^(25^ 100 Hi
SaTd Vapor (0.5 atm) it
Sohtbiity of ««tr it 7(rr (2U*CX X by wt
Solubility in wattr at saturation pressura < TtTF
(21.lt) % by wt
Oifnjswity in sir at 7TF (2S*C) and I atm, cn*/ssc
ft1/hour
Toiicrry
(TWM»pm)
0.4619
7J99
S3.12
3SJI7
(L213
0.152
(L043
0.00430
0.694
00102
L355
17J
4.4
2.41
1JJ10
0.009
0.017
OJKI
0.264
1000
0 20 40 *0 SO 100 1M 140 1*0 ISO 900
TSMfVATUM. *P.
FIGURE 2 Vapor Pressure vs. Temperature
too
•0
0 10 M M 40 SO M 70 M 110 130 ISO
300
Figure 3 gives psycfarometric curves for "Freon" TF vapors
in air. At room temperature, one pound of air is capable of
holding four pounds of "Fnon" TF vapors. The tremendous
appetite of air for -Ficon" TF means that drying will take
place rapidly at room temperature. In forced air drying sys-
tems or ventilation systems, the size and cost of air handling
equipment is kept to an absolute minimum.
SELECTIVE 'SOLVENT POWER
An outstanding advantage of "Freon" TF is its abihty to
dean without ^iMgfag any of toe materials of construction
of the article being dsened. It • selective in its cleaning acuon
because it wul dissolve or flush away the contaminants on the
article and yet wul not attack metals, plastics, or elastomers.
Table II gives typical guJdeposn on the compatibtlm of
"Freon" TF with a variety of materials. In general it B com-
pletely mtscibte with petroleum hydrocarbons, chkmruied
hydrocarbons, lower aliphatic alcohols, ketones, ethers, esters.
animal, vegetable and mineral oils.
Thus "Freon" TF is compatible with most organic systems.
When they are present on articles, as soils or contaminants,
"Freon" TF wul remove them leaving a residue-free surface.
Most of the materials in the "miscibfc" column are also
cleaning media. "Freon" TF can be substituted for these in
most cases or used as a final cleaning step to remove tracts of
these cleaning media or residues they leave behind.
-------
FIGURE 3 PsydirofiMtric Chart
'
It
17
11
12
10
f
I
r
*
s
4
3
I
1
, J'FIEON" TF VAPO* IN All;
AT ATMOSFHUIC FtESSURt
fee***".
"%}&/•&&*$*&£•?* ,
-r "-••• •.••"'••"• -:v^?s- I]
... _^.;.:/.._. .. j/.^i,^;. 5J
MT tuu numKAnitf. •*.
The solvent power of "Freon" TF k intermediate between
aliphatic hydrocarbons and chlorinated hydrocarbon solvents.
_ Since there is no single scale which can rate solvent power on
)> an absolute basis, it is always recommended that specific sot-
vent tests be run for a specific soil However, a general guide
,, » relative solvent ratings can be obtained by the OM of
Kauri-Butanol (KB) numbers and sohibflity parameters.
These guides are two independent empirical systent for esti-
mating solvent power and are given in Table in for a number
orsolvents. In general, the higher the munben on these sol-
vent scales, the stronger the solvent. In actual practice then
an many exceptions to the relative ratings suggested by these
guides. Solvent power is only one of a number of physical and
chemical factors involved in the selection of a cleaning agent.
It should be used only for the purpose of the crudest possible
screening of candidate cleaning materials.
Table III. Guides to Relatfv«~'
Solvent Power~
Kaurl-Butanol Solubility
aoiwrn nunia«r rarwnvnr
Kerosene
"Freon" TF
n-Heptan*
Stoddard Solveirt
"Freon" TA
"Freon" TMC
Benzene
1.1.1-Triehloroethane*
Trichloroathylene
Methytone Chloride
Chloroform
29
31
35
37-39
51
86
105
120
130
136
208
7*
72
7.4
7.4-7.5
—
—
9.2
—
9.3
9.7
9.3
inallul nMnmfnrm
EFFECT ON MATERIALS OF CONSTRUCTION
A clear-cut distinction must be made between the following
when using the term "materials of construction" hi rfainhig
applications:
1. The materials used in construction of the article being
cleaned which is exposed for relatively brief time inter-
vals to the cleaning agent under, a specific set of
conditions.
2. The materials used in construction of the cleaning
equipment which involves continuous exposure to the
solvent under a variety of conditions.
With few exceptions "Freon" TF can be used to dean
articles made of any material of construction. However, clean-
ing equipment construction materials should be selected to
withstand an use conditions, ^r"1*"" steel is the most com-
monly used construction material
Table II. Solubility of Various Substances in
"FREON" TF Solvent at Room Temperature
Misctbto
Moderately Soluble
Slightly Soluble
Insoluble
Acetone
Benzene
Carbon Tetrachlortde
Ckl^M^MMW
nwfvforni
Diethyl Ether
Ethanol
Hexane
Kerosene
Methyl Alcohol
Mineral Oil
Ethyl Acetate
Azobeflzene
Benzophefwne
Camphor
Cocoa Butter
Cottonseed Oil
Naphthalene
Thymol
Trlbromophenol
Silteone Oils
AcstanilM*
BenzJI
Benzole Acid
Diphenyl
Oiphenyl Carbinol
Ester Gum
Hexachtoroethane
Pnthalic Anhydride
Stearto Acid
Paraffin Wax
(MP 126T)
Aoatamide
Antnric0n<
Gum Mastic
1 n ft nMn f^n
Ivwwvvffl
Phenol
Salicylic Acid
TartartcAcId
Urea
Paraffin Wax
(MP 141«F)
Agar
Caeein
Canutes* Acetate
Oetatin
Nitrocellulose
Shellac
Starch
Sugar
Water
Gryceral ft Most
Polyhydric Alcohols
'WON to 0»
-------
SAFETY
-Tram" TF is not flammable or explosive
and has no flash point To illustrate the beneficial effect of
"Freon" TF solvent's nonflammable characteristics, a num-
ber of flammable solvents were blended with "Ficon" TF
at various ooocenusrieni, Data in Table XIV show the
extent to which "Freon" TF elevates the initial flash point
of these other solvents. It must be borne in mind, however.
that "Freon" TF may hare a higher rate of evaporation
than the flammable solvents. Consequently, if a significant
amount of evaporation occurs, the flammability property
of the mixture, as measured by flash points, tends to return
to the more hazardous condition. Generally, however, some
beneficial elevation of initial flash point is usually retained,
at least until more than 50% of the blend has evaporated.
Table XIV. Effect of "FREON" TF In
Suppressing Flash Points of
Flammable Solvents • •- -
Initial Flash Point *f*
"Freon" TF Weight % "Freon" TF in Blend
Blended with 0 10 20 30 40 60
Acetone
Ethanoi
Toluene
VM4P Naphtha
3 36
55 100 115
40 83 103
35 46 57
70 104
120
107
67 72
Stoddard Solvent 150 155 178
Mineral Spirits 130 147 165
•Ctavotantl Opon Cup
182
Toxidty—"Freon" TF is low in toxkity and its TWA (8-
hour Tune-Weighted Average value), as calculated accord-
ing to OSHA procedures, is 1.000 ppm. This is the maximum
Time-Weighted Average vapor concentration allowed by
OSHA regulations for continuous exposure of workers hi
an eight-hour day, 40-hour week.
"Freon" TF solvent is less toxic than most other commer-
cial solvents (see Table XV) and therefore can be used with
fewer restrictions; but as with all solvents, inhalation of
high concentrationsjs daflfvoos and can prove fatal Any>
one suffering from the uo£ effects of the vapor should im-
mediately move or be asjjjfpd to fresh air. When treating
persons suffering toxic effects due to exposure to vapors of
"Freon" TF and most other commercial solvents, the use
of tpinephrine and similar drugs should be avoided be-
cause they may produce cardiac arrhythmias, including
ventricular fibrillation.
In most plant situations, existing ventilation systems may
be adequate for keeping "Freon" TF vapors at a safe con-
centration (less than 1,000 ppm).* However, each and every
case should be scrutinized carefully to make sure that
•*ood safety practice is being followed. Special ventilation
nould be provided in work areas where high concentra-
tions are likely to occur (e.g. spraying operations) and in low
places where heavy vapors may collect Storage tanks, vapor
degreascrs, and other confined spaces must not be entered
(even if only for making an inspection) without observing
standard safe tank entry procedures.
.
Tabje_XV. 8-Hour Time-Weighted Average
JT-.III *Aeheaa««fc>-_iv - -•- .. «*• » * — . • fc •: *.' »**
Concentrations for Some^C?:
Common Solvents' as Allowed * '
by. Occupational Safety and- ^
Health Administration — -,
Substance *
"Freon" TF
Ethyl alcohol
Hexane
Stoddard solvent
Methytene chloride
1,1.1 Trichloroethene (Methyl ehlorol
rvrcnioroemyMne
Trichtoroethylene
Benzene
Carbon Tetrachloride
TWA1
(ppm)
1,000
1.000
500(100)*
500(100)*
500K100)*
term) 350
100*
100*
50*(10)»
10*<10)»
1. tipnmtt •• pvti ptr MMtan * vapor In cmnnlimu itr
mtutc OMte» M aS*C «nd no mm Hf gnmun. (So* Co* of
^•gmtucitt, as (Ubor). PM§ isoo M isit (My. itit).
2. Th»»»
1. MmKxr» to
|.
Binngiini M ThrMkeM UnN VafeM OLV« ta ppw)
M Ittl by •»• AiMricjo ContocMM of Qo»^n<^n<»<
The preceding information shows that "Freon" TF is
unique among commercial solvents because it is both ooo-
fiainmable and. low in toxictty. To our knowledge there have
been no implications to date of caxctoogenicity, mutagenic-
iry.orteratofeakiryajsociatedwUitrichlcfocrinuo^
in animal studies and human experience. A summary chart
comparing these safety properties with other solvents is given
in Figure 4.
The Du Pont Company and its authorized agents will
gladly supply •fr't^ntt in analyzing use conditions and in
specifying equipment, handling and monitoring procedures
needed to assure safe operation with "Freon" TF solvent
Deeoeapo«lne«—Although "Freon" TF solvent is non-
flammable and will not support combustion, it can be de-
composed by open flame or hot surfaces such as inr space
heaters, The decomposition products are corrosive and
toxic, but they an so irritating mat persons working in
their presence find them almost impossible to ignore. Good
ventilation minimizes hazards from decomposed solvent
Concentratiom of "Freon" TF vapors wen below the
TWA level win, in time, severely damage space healers if
vapors an drawn into the healer combustion area. Pro-
vision should be made for an indrpcnoVnt supply of air or
the use of another type of heating system.
SUn and Ey» Contact—If "Freon" TF is splashed in the
eyes, it may cause irritation. Should this occur, immediately
flush the eyes with water and obtain medical attention.
Since "Freon" TF dissolves natural ofls, it may lead to
skin cracking and irritation. Prolonged contact should be
avoided. Hands should be protected with neoprene gloves
if prolonged or repeated contact is expected. Clothing that
becomes wet with "Freon" TF should be removed at once.
-------
MnmuMt CMMBBC
I
NAFHTMA
noooAto sotvwt
mm
earth metals neb as sodium, potassium, and barium ia their
free metallic form. These materials become more reactive
when finery 'ground or powdeied and, in this state, mag-
nesium and aluminum may react with fiuorocarbons espe-
cially at high temperatures. Highly reactive materials
should not be brought into contact with fluorocarboos until
a careful study is made and appropriate safety precau-
tions an taken.
ENVIRONMENTAL AND OCCUPATIONAL LEGISLATION
"Preen" TF is a saturated fluorocarboo and is not photo-
chemkaDy reactive. This b reflected in minimum restrictions
on its use imposed by federal and stale regulations under the
dean Air Act of 1970, and the Environmental Protection
Agency.
The tow order of toxiehy and general safety inherent in the
us* of "Freon" TF provides a wide margin of safety for
employees and racilitates compliance with the Occupational
Safety and Health Act of 1970 (OSHAX
SPECIFICATIONS
Ecuiototvi
TtnAMVOaOWSAN
Appearance
ComposWan (by weight)
TriduoroWfluoroethsne
Chloride ion, expressed as a
Moisture (by weight)
Acidity (mg KOH per gram of sample)
Residue (Soluble and (insoluble, combined)
(by weight)
deer color-
less liquid
99.80% min.
0.1 pom max.
lOppm max
0.003 max,
2 pom max.
"Freon" TF should not be taken internally.
Reactivity—Those doing unusual experimental and devel-
opmental work with "Freon" TF should be aware that
fluoracarbons, like other hatocarbons, may react violently
with highly reactive materials, including alkali and alkaline
PACKAGING AND AVAILABILITY
Treon" TF solvent is available in 5- and 55-gallon drums
and in tank truck and tank car quantities. Prompt delivery
is assured by the easy availability of many Authorized
Distributors located throughout the country.
NOTES
FftfON M On *•*•• «••**•<•« tndMMrt tar Hi •Miacartin ce«i»«ui>di
-------
Table 2. Soil Washer Laboratory Feasibility Study Experimental Summary
Starting Concentration of Native TCDD on Soil is 671 ng/g
Tl
loluene/IPA
4:1 v/v
Freon
Freon/MeOH
4:1 v/v
Diesel Fuel/
M^O
4:1 v/v
Kerosene/H^O
1 :4 v/v
H20
It NP 90
IX Adsee 799
21 HP 90
2i Adsee 799
31 NP 90
31 A.lsee 799
Stage 1
Stage 2
Stage 3
Stage 4
(Wash)
Stage b
(Residue by Soxliltl )
» 1
* !
1 4
^ 1
#3 2
7 1
P 2
1 1
•0 2
'1 1
'2-2
'3 1
'< 2
// ,
iV-2
n 3
IP 4
'•» 1
?o 2
'*4 3
un
2-3 i
•M?
85
89
75.9
78.1
76.6
76.2
76.5
81.2
64.5
60.0
52.9
46.1
0.05
0.06
18.4
45.2
32.4
35.0
60.5
51.1
55
54
57.0
57.3
100
74
162
147
157
160
158
122
238
268
316
362
671
671
548
368
454
436
268
325
302
309
288
286
85.0
89.0
75.9
78.1
76.6
76.2
76.5
81.2
64.5
60.0
52.9
46.1
0.05
0.06
18.4
45.2
32.4
35.0
60.5
51.1
55
54
57.0
57.3
10.9
11.0
14.3
12.1
13.0
13.4
14.2
9.2
24.3
25.6
20.2
19.6
25.0
20.5
20.5
NA
89
73
61
78
70
36
221
300
384
196
130
197
134
171
151
86.8
89.1
90.9
88.3
89.5
94.6
67.1
55.3
42.7
70.8
80.7
70.7
80.0
74.5
77.5
NA
1.6
1.6
4.1
4.1
1.4
1.5
5.3
4.4
26.1
18.1
4.8
7.5
7.0
5.2
5.8
NA
79
62
33
51
61
26
185
270
209
74
97
146
87
136
112
88.4
90.7
95.0
92.4
90.9
96.1
72.4
59.7
68.8
88.9
85.5
78.2
87.0
79.7
83.3
NA
12.4
13.3
7 3
7.6
3.0
2.8
'
21.5
NA
2.3 194 71.1 27.6
1.9 62 90.8 26.8
2.77 78 88.3 NA
2.65 128 80.9 NA
1.78 75 88.8 22.1
1.75 124 81.5 20.1
1.2 104 84.5 13.2
NA NA NA
83
89
49
51
21
19
144
IBS
ISO
148
133
08
101
104
102 3
100
93 9
9B.9
93.9
NA
go.;
117.6
NA
NA
110.9
101.4
9;.;
NA
-------
Table 2 Soil washer Laboratory Feasibility St.idy Experimental Sugary
Starting Concentration of Native TCDD on Soil is 671 ng/g
A,
lolnene/lPA
4:1 v/v
Freon
Freon/MeOII
4:1 v/v
Diesel Fuel/
1120
4:1 v/v
Kerosene/MzO
1:4 v/v
II20
|I NP 90
IX Adsee 799
21 HP 90
21 Adsee 799
31 HP 90
31 Adsee 799
Stage 1
Stage 2
Stage 3
Stage 4
(Hash)
Staqe 'j
(Des nine l>y Soxlilcl )
* 1 85
^2 89
9 3 75.9
"[ 4 78. 1
^ 1 76.6
"=• 2 76.2
71 76.5
(,' 2 81.2
9 1 64.5
'0 2 60.0
'1 1 52.9
'L~2 46.1
'3 1 0,05
'4 2 0.06
'* 1 18.4
l<,2 45.2
r/ 3 32.4
IP 4 35.0
'1 1 60.5
7°2 51.1
^ 3 55
24.4 54
^-3 1 57.0
2.<,2 57.3
100 85.0
74 89.0
162 75.9
147 78.1
157 76.6
160 76.2
158 76.5
122 81.2
238 64.5
268 60.0
316 52.9
362 46.1
671 0.05
671 0.06
548 18.4
368 45.2
454 32.4
436 35.0
268 60.5
325 51.1
302 55
309 54
288 57.0
286 57.3
10.9
11.0
14.3
12.1
13.0
13.4
14.2
9.2
24.3
25.6
20.2
19.6
25.0
20.5
20.5
NA
89
73
61
78
70
36
221
300
384
196
130
197
134
171
151
86.8
89.1
90.9
88.3
B9.5
94.6
67.1
55.3
42.7
70.8
80.7
70.7
80.0
74.5
77.5
NA
1.6 79
1.6 62
4.1 33
4.1 51
1.4 61
1.5 26
5.3 185
4.4 270
26.1 209
18.1 74
4.8 97
7.5 146
7.0 87
5.2 136
5.8 112
NA
88.4
90.7
95.0
92.4
90.9
96.1
72.4
59.7
68.8 2.3
88.9 1.9
85.5 2.77
78.2 2.65
87.0 1.78
79.7 1.75
83.3 1.2
NA NA
194
62
78
128
75
124
104
12 4
13.3
7.3
7.6
3.0
2.8
21.5
NA
71.1 27.6
90.8 26.8
88.3 NA
80.9 NA
88.8 22.1
81.5 20.1
84.5 13.2
NA NA
83
89
49
51
21
19
144
185
180
148
133
88
101
104
102 1
100
93.9
on. 9
93.9
NA
98.7
117.6
NA
NA
110.9
101.4
97.7
NA
-------
Table 2. Soil Washer Laboratory Feasibility Study Experimental Summary
Starting Concentration of Native TCDD on Soil is 671 ng/g
Stage 4
(Hash)
Stdy SnxMt-l )
Toluene/I PA
4:1 v/v
freofi -i
K J
rreon/MeOII 7
4:1 v/v tf
Diesel Fuel/ 9
11^0 'C
4:1 v/v
Kerosene/H^
1:4 v/v
11^0
21 NP90
21 Adsee 799
3% HP 90
31 Adsee 799
'1 1
'1-2
|X NP 90 tf 1
|X Adsee 799 \(, 2
rf 3
if 4
^ 3
ii.4
76.
76.
76.
81.
64.5
60.0
52.9
46.1
0.05
0.06
IB.4
45.2
32.4
35.0
60
51
55
54
57.0
57.3
157
160
158
122
238
268
316
362
671
671
548
368
454
436
268
325
302
309
288
286
76.6
76.2
76
81
64.5
60.0
52.9
46.1
0.05
0.06
IB.4
45.2
32.4
35.0
60.5
51.1
55
54
57.0
57.3
14.3
12.1
13.0
13.4
14.2
9.2
24.3
25.6
20.2
19.6
25.0
20.5
20.5
HA
61
78
70
36
221
300
384
196
130
197
134
171
151
90.9
88.3
(19.5
94.6
67.1
55.3
42.7
70.8
BO. 7
70.7
80.0
74.5
77.5
NA
4.1
4.1
1.4
1.5
5.3
4.4
26.1
18.1
4.8
7.5
7.0
5.2
5.8
NA
33
51
61
26
185
270
209
74
97
146
67
13G
112
95.0
92.4
90.9
96.1
72.4
59.7
6B.8
BO. 9
85.5
78.2
87.0
79.7
83.3
HA
2.3
1.9
2.77
2.65
1.78
1.75
1.2
NA
194
62
78
128
75
124
104
71.1
90.fi
88.3
BO.9
88.8
81.5
84.5
HA
7.3
7.6
3.0
2.n
21.5
NA
27.6
26. B
NA
NA
22.1
20.1
13.2
NA
49
51
21
19
141
ins
I no
148
133
88
I02.3
UK)
91.9
911.9
9J.9
NA
W.I
NA
NA
110.9
101.4
97.7
NA
-------