HomeMy WebLinkAboutSmuggler Superfund- Lead Speciation Study 1992, Lab Svs at Smuggler CERCLA SITE Ph 1Thomas S. Dunlop, Director
Aspen/Pitkin €nvironmental
iealth Department
130 S. Galena
Eespen, GC? 81611
LABORATORY SERVICES AT
SMIIGGLER MOIINTAIN CERCLA SITE
ASPEN, COLORADO
IIRS CONSIILTANTS
DEPARTMENT OF GEOLOGICAL SCIENCES
IINIVERSZTY OF COLORADO
CAMPIIS BO% 250
BOIILDER, COLORADO 80309
PHASE I
OCTOBER 23, 1992
PREPARED FOR
SIIBCONTRACT IINDER IIRS CONSIILTANTS
INTRODIICTION
Nineteen solid samples from the Smuggler Mountain CERCLA site,
Aspen, Colorado were provided by URS Consultants on Suly 30, 1992
via Federal Express ( see Appendix I for a copy of airbill #
3821503140j. The nineteen samples submitted for analyses were
collected by URS, locations are given. in Figure 1. Sample
character, and descriptions were not provided, and we cannot
respond to sample quality nor to the degree to which they may or
may not represent the study area.
The purpose of this-study was to determine the speciation of lead-
bearing phases in each of the samples for an assessment:. of
bioavailabilty. The term speciation in this report is meant to
refer to the form(s) of lead and their frequency of occurrence in
each sample. Bioavailability of the lead will be characterized
based on such factors as; lead species (stoichiometry), grain-size,
and associations. Associations refer to the mode of occurrence of
the lead-bearing phase ie. is it INCLOSED within a .non-lead
mineral, is it RIMMING another mineral, is it CEMENTING or
ENCRUSTING other mineral(s), or is it free within the soil MATRIX.
SAMPLE PREPARATION AND ANALYSIS
Approximately 1.O grams of air-dried material from each sample was
mounted in epoxy for polishing and microscopic examination. Details
of mounting and polishing are given in Appendix I.
2
Samples were analyzed on a JEOL 8600 Superprobe located in the
Department of Geological Sciences, University of Colorado, Boulder,
Colorado. A combination of EDS (energy dispersive spectrometry),
and WDS (wavelength dispersive spectrometry) along with the aid of
a backscatter electron detector were used in this study to isolate
and identify the lead-bearing phases.
Operating conditions include a 15Kv accelerating voltage, 20-30
NanoAmp cup current and a 1 micron beam size. Wavelength
spectrometer crystals: LIF-PET for lead, PET for sulfur, LDE1 for
oxygen, and LDEC for carbon were used in analyses. To ensure a high
degree of accuracy in the microprobe analyses spectrometers were
peaked daily and mineral standards were analyzed randomly as
unknowns. Calculated accuracies ranged from 1 to 5 percent of the
amount determined and MDL's (minimum detection limits) ranged from
0.01 to 0.03 wt~.
Point counts were made on each sample until a total of at least 100
lead-bearing particles were identified or 8 hours scanning time was
reached. Particles were isolated by traversing each sample from
left-to-right and top-to-bottom at a low magnification 40-100X and
then at a higher magnification 200-600X.
ELECTRON MICROPROBE ANALYSES
Nearly 70~ of all the lead-bearing phases found in this set of
samples are found to be cerussite or FePb oxide, Figure 2.
cerussite tends to be found free within the matrix or encrusting
other silicate minerals. It also often rims galena particles.
cerussite still accounts for more than half of the total bulk lead
ro
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ASPEN
URS
Pb Bar
Ga
Pb Org
Ang
Pb Phos
MnPb Ox
FePb Ox
FePb Sulf
Cerr
0 5 10 15 20 25 30 35 40 45 50
LEAD PHASE FREQUENCY
BURM -RESIDENTIAL SOILS
FIGUP.E 2
1
y ~
C
within the samples. FePb oxides ,have variable lead contents,
ranging from 1 to 28 percent. They are free with the sample matrix
or form as cements or coatings on other silicate phases.
The remaining 30~ of the lead-bearing population 'is predominahtly
composed of FePb sulfate, and MnPb oxide.. The MnPb oxide is .most
often found free within the matrix or as cements. FePb sulfate is
usually free within .the matrix or found rimming pyrite grains.
The data indicates. that approximately 90% of -the lead-bearing
phases. counted fallbetween 1 and 20 microns.. The. largest
proportion of grain's within this, size range are found free within.
the sample matrix. Only one phase, .galena, illustrated an
association which would limit its bioavailability; the other lead-
bearing phases should be considered .available. Microprobe analyses
of other silicate grains does suggest that a VERY thin (1 to 50
angstroms) coating of FePb oxide may be common; however, this would
not.. represent a very significant portion of the lead pool.
LEAD BIOAVAILABIL.ITY AS IT RELATES TO SPECIATION
Lead uptake, through digestion or inhalation, in these samples is
likely controlled by the minerals;. cerussite, Fe-Pb oxide, Fe-Pb
sulfate, and Mn-Pb oxide. Although .galena is common in some. of the
samples, (particularly the coarse fraction), these are generally
rimmed by cerussite or in rare cases anglesite and therefore not
likely to be a significant contributor to. the lead-pool when the
material is digested. cerussite is likely to be the most
F
significant phase for four reasons: 1) it is the first or second
most abundant lead-bearing phase, 2) it contains 77 to 80 percent
lead by weight, compared to Fe-Pb oxides, Mn-Pb 'oxides and Fe-Pb
sulfates which range from 2 to 50 percent lead by weight, 3) its
morphology has a much higher surface area of exposure (increasing
solubility), 4) the Fe-Pb oxides and Mn-Pb oxides are generally
larger in size and therefore less likely to be digested or inhaled.
a
PHASE FC-003-250 FW007 250 RW008-250 if
Cerussite 12%8::14%3 43%3 :_.
FePb 4%6~10%3 10%2Sulfate
FePb Oxide 61%11:64%4 ..29 %3 .::
MnPb Oxide 17%10':12%3 4 %1 .!:
Pb 1%7::1%l
Phos hate
An lesite 5%8 €4 %1
Pb Or anic 5 %1 .,
Galena 7%2
Total
Particles
28 233 391
PHASE RH001-250 RW001-250
FePb Oxide 70%5 77%3
Cerussite_7%5 3%2 ':
FePb Sulfate 2%2 Tr
MnPb Oxide 15%5 20%4
Pb Phos hate 4$3 Tr
Pb Or anic 3%3
Total 117 224
Particles
TABLE 1. Compilation of lead-bearing phase mineralogy for the Smuggler
URS sample set. Estimated error at the 90% confidence level
based on the Normal distribution error curve.
8
PHASE RH003-250 f- -RH002-250 i• -
Pb Or anic 9%i 2 ':1%1
Cerussite 26%4 31%3__
FePb Oxide 37%4 34%3
FePb Sulfate 8%2 !11%2
MnPb Oxide 13%3 10%2
Galena 3$2.3%1
An lesite 3%2 ' +9%2
Pb Phos hate 3%1 :
Total 270 513
Particles
PHASE FW004-250 RH004-250
Pb Barite 2%6
MnPb Oxide 3%6
FePb Oxide 40%6 33%23
FePb Sulfate 12%10 2%5
Cerussite 12%10 39%12
Galena 3%6
CuZnPb 21%12
PbCl 1%5
Total 20 27
Particles
TABLE 1. Cont.
9
y
PHASE FW003-250 t FW002-250 i-
An lesite 2%2
Pb Phos hate 31%6 14%9 ::
FePb Oxide 42%6 36%12z
Galena 1%2 1%7< i
MnPb Oxide 15%5 47%13<.
FePb Sulfate 3%3
Cerussite 5%4 2%5
PbCL 1%2
Total 100 25
Particles
PHASE FW006D 250 F FW006-250
Cerussite 20%4 7%2
Pli Or anic 1%2
Pb Phos hate 6s 2 10%2
FePb Sulfate 17%4 11%3
MnPb Oxide 5%3 10%2
FePb Oxide 49%5 62%4
An lesite 1%s 2
Total 157 295
Particles
TABLE 1. Cont
io
Total I 61 I I 9
Particles
PHASE FH001-250 FH002-250
FePb Oxide 32%3 60%2
Pb Or anic 7%i
Cerussite 27%3 16%2
FePb Sulfate 21%2 13%2
MnPb Oxide 7%1 9%2
Galena 4%I 1%1
Total 572 609
Particles
PHASE FC001-250 FC002-250
FePb Oxide 56%7 46%20
Galena 1%3 1%9
MnPb Oxide 7%5
Cerussite 1%3
Pb Barite 9$g
Pb Phos hate 26%7
FePb Sulfate 1%3 52%19
TABLE 1. Cont.
11
PHASE RH005-250 t-RW005-250 t- -
Cerussite 30$2 49$5
FePb Oxide 30$2 32$5
FePb Sulfate 17$2 2$2
MnPb Oxide 10%2 6$2
Galena 4%1 8$3
Pb Or anic lOg 2
Pb Phos hate 2$1
Total 597 180
Particles
TABLE 1. Cont.
12
IIRS and CDM COMBINED SAMPLING
In the combined URS and CDM program I was able to study 28 samples
from the Smuggler Site, representing the 0 to 2 inch depth
interval. In these samples over 18,000 lead grains were identified
ahd counted. The normalized (based on total particles counted)
frequency for the site as understood at the time of this report is
illustrated in Figure 3. FePb oxide and cerussite are
overwhelmingly the most common lead-bearing phases with cerussite
dominating the lead source pool. Most (90%) of the lead-bearing
particles in these sieved samples fall within the 1 to 10 micron
grain size.
Only minor differences in mineralogy are noted in the burm and soil
samples. This is not what I would have anticipated; however, it may
be due to the fact that we are ONLY looking at the 0-2" depth
interval were mineralogy is controlled predominantly by oxidation.
Burm samples show a distinctive increase in FePb sulfate along with
an absence of anglesite and Pb phosphate.
The site has a crude zonation from NE to SW:
NE ++ Galena, Anglesite, cerussite
FePb Oxide, cerussite
SW ++ Pb Phosphate, MnPb Oxide
cerussite
s
13
Pb Phosphat
Fe-Pb Sulfat
z Mn-Pb Oxid
w Fe-Pb Oxid
m
Q°Anglesit
w
Galen
O
Cerussite
SMUGGLER MINE
Aspen, Colorado
v ~u 30 40 50
5 15 25 35 45
NORMALIZED FREQUENCY
CDM Soils ~ URS Soils Burm
e
e
e
e
e
a
FIGLRE 3
14
This zonation reflects the movement away from the mines into an
area with increase residential input; ie. soils and fertilizers.
Mineralogically galena is the only lead-bearing phase that should
be excluded from the total lead pool due to its consistent lack of
bioavailability. Clay or silicate coatings are found on some lead-
bearing phases; however, I would estimate this to be only about 20-
25 °s of the time and seldom complete. Many times lead-bearing
grains are closely surrounded by. other silicates; however,
significant void space can be found between these grains and
although this may deter fluid movement it will not restrict it.
14C
120
U
100
80
u_
w
60
a
p 40
Q
w
J
ASPEN
URS
SAMPLE RW008-250
Pb Org 5%
FePb Sulfate 10%°
Cerussite 43%
Galena 7%
Anglesite 4%
FePb Oxide 29%
MnPb Oxide 4%
5 ~ 10 20 30 50 75 100 0 20 250
GRAIN-SIZE Microns
ASPEN
URS
U
Z
w
O
w
w
w
a
0
w
140
120
100
80
SAMPLE RW-001-250
Pb Phos Tr
Cerussite 3%
FePb Sulfate Tr
MnPb Oxide 20%
FePb Oxide 77%
5 10 20 30 50 75 100 150 200
GRAIN-SIZE Microns
ASPEN
U RS
o
60
U
w 50
C~
40
u_
w
Q 30-
d
0 20-
w
10-
SAMPLE RW005-250
MnPb Oxide 6%
FePb Oxide 32%
Cerussite 49%
Galena 8%
Pb Phos 2%
FePb Sulfate 2%
ASPEN
URS
U
Z
w
O
w
w
w
o_
0
Q
w
350
SAMPLE RH005-250
Cerussite 30%
150
1
FePb Oxide 30%
FePb Sulfate 17%
MnPb Oxide 10%
Galena 4%
Pb Org 10%
5 10 20 30 50 75 100 150 200 250
GRAIN-SIZE Microns
ASPEN
URS
1
w 1
C~
w
u:.
w
Q
a_
Q
w
J
3-i
SAMPLE RH004-250
FePb Oxide 33%
Pb Phos 25%
Cerussite 39%
FePb Sulfate 2%
PbCI 1
a iv GU ~U bU /5 100
GRAIN-SIZE Microns
ASPEN
URS
120
SAMPLE RH003-250
100
Z Pb Org 9%
w
80 Cerussite 26%
Q
w
FePb Oxide 37%
60w
cn FePb Sulfate 8%
n- 40 MnPb Oxide 13%
w Galena 3%
J
20
Anglesite 3%
5 10 20 30 50 75 100 150 200 250
GRAIN-SIZE Microns
300
U 250
z
w
200
w
w 150
o=..100
0
w
sn
ASPEN
URS
GRAIN-SIZE. Microns
ASPEN
URS
U
Z
W
Cl
w
w
w
2
o_
0
w
J
35
15
10
5
0
5 10
SAMPLE RH001-250
20 30 50 75 100
GRAIN-SIZE Microns
FePb Oxide 70%
Cerussite 7%
FePb Sulfate 2%
MnPb Oxide 15%
Pb Phos 4%
Pb Org 3%
150 200 250
120
100
U
Z
W
80
W
W
w 60:
Q
a-40
0
w
J r„~
0
ASPEN
URS
SAMPLE• FW007-250
ASPEN
URS
U 50
z
w
0 40
w
m
u_
30w
Q
20
0
w
10
0
5 10
Sample FW006D-250
Cerussite 20%
Pb-ORG 1
Pb Phos 6%
FePb Sulfate 17%
MnPb Oxide 5%
FePb Oxide 49%
Anglesite 1
20 30 50 75 100 150
GRAIN-SIZE Microns
ASPEN
URS
200
180 SAMPLE FW-006-250
U 160
Z
w 140
G~Cerussite 7%
w 120
Pb Phosphate 10%
w 100
FePb Sulfate 1180
60 MnPb Oxide f0%
0
Q
40 FePb.Oxide 62%
20
0
5 10 20 30 50 75 100 150 200
GRAIN-SIZE Microns
ASPEN
URS
1
z 8
w
Q
6_
u..5w
ar
4-
w
3-0
w 2-
J
1-
0-
Sample FW004-250
5 10 20
GRAIN-SIZE Microns
Pb Barite 2%
MnPb Oxide 3%
FePb Oxide 40%
FePb Sulfate 12°/a
Cerussite 12%
CuZnPb 21%
Galena 3%
30
ASPEN
URS
60
5U
U
Z
w
Q 40
w
w 30
20
0
Q
w
10
0
SAMPLE FW003-250 Anglesite 2%
Pb Phos 31
FePb Oxide 42%
Galena 1
MnPb Oxide 15%
FePb Sulfate 3%
Cerussite 5%
PbCI 1
5 10 20 30 50 75 100
GRAIN-SIZE Microns
ASPEN
URS
U
Z
w
Q
w
v_
w
Q
a_
D
w
f SAMPLE FW002-250
Cerussite 2%
0
Galena 1%
FePb Oxide 36%
Pb'Phas 14%
MnPb Oxide 47%
3
5 1 U "LU ~U 5U
GRAIN-SIZE Microns
ASPEN
URS
450
400 Sample FH002-250
z 350 FePb Sulfate 13%
w
O 300 Cerussite 16%
w
250 MnPb Oxide 9%
Q 200 FePb Oxide 60%
0 150 Galena 1
w 100
J
0
5 10 20 30 50 75 100 150 200
GRAIN-SIZE Microns
Q
ASPEN
URS
SAMPLE FH001-250
FePb Oxide 32%
Pb Org 7%
Cerussite 27%
FePb Sulfate 21
MnPb Oxide 7%°
Galena 4%
5 10 20 30 50 75 100 150 200 250
GRAIN-SIZE Micronns
ASPEN
URS
1
U 1
z
w
d
w
a=
w
L~
z
w
m
0
w
J
Sample FC-003-250 FePb Sulfate 4%
Cerussite 12%
FePb Oxide 61
MnPb Oxide 17%
Anglesite 5%
Pb Phos 1
5 10 20 30 50 75
GRAIN-SIZE Microns
ASPEN
URS
Galena 1
FePb Oxide 46%
FePb Sulfate 52%
5 10 15 20 30
GRAIN-SIZE Microns
50
U 35
z
w
30
C3
w
ct 25
u_
cwn 20
Q
a- 15
0
w 10
J
5 10
ASPEN
URS
SAMPLE FC001-250
FePb Oxide 56%
Galena 1
MnPb Oxide 7%
Cerussite 1
Pb Barite 9%
Pb Phos 26%
FePb Sulfate 1
20 30 50 75 100 150
GRAIN-SIZE Microns
PHOTO I. Backscatter photomicrographs from sample FH002-250
illustrating typical associations:. A) FePb oxide
cementing silicate matrix B) compound grain of MnPb
oxide rimmed by later FePb oxide.
PHOTO 2. Backscatter photomicrograph illustrating crystallization
of late Pb phosphate in silicate fractures from sample
FC001-250.
a
SU0i~2TQOSSE
a~tsaTbue ~uaTpb (g pua a~tsaZbuE e~TSSnzao
bar~pz~snjZt OSZ-EOOH2i aZd~2s uoz3 ud2zbozaT~o~ogd '£,OSOHd
OSZ-£OOH~ aTd~Qg •a~tssruao ~q 2uajeb ;o buTmiutz
aq~ (g put a~tssnzao oq uoamtoo eaza aoe3zns antsuagxa
auk (y :but}ez~snTTt gdezbozot~ogoqd zaq}eosxo2g ••y OSOHd
PHOTO 5. Photomicrograph .from sample RFI003-250 of lead-bearing
organic matter.
PHOTO 6. Backscatter photomicrograph from sample RH003-250
illustrating alteration of cerussite to FePb oxide.
PHOTO 7. Backscatter photomicrographs from sample RW005-250
illustrating: A) alteration of galena-cerussite-FePb
sulfate B) and cerussite to FePb oxide.
9
PHOTO 8. Photomicrograph illustrating alteration of galena to
cerussite. Note increase surface area created by
cerussite formation. Sample RW005-250.
PHOTO 9. Backscatter photomicrograph from sample RW0o8-250
illustrating the formation of FePb sulfate from pyrite
oxidation.
9
PHOTO 10. Backscatter photomicrographs from sample RW008-250
illustrating typical associations for cerussite: A)
large, isolated grains in matrix and B) cerussite rimmed
incompletely by FePb oxide.
PHOTO 11: Backscatter photomicrograph from sample RH005-250 of
lead-bearing organic matter. Note how the lead is
confined to the outer 10 micron rim.
PHOTO 12. Backscatter photomicrograph from sample RH005-250 of
small FePb sulfate grains with cerussite.
PHOTO 13. Photomicrographs from sample FW003-250 of various Pb
phosphate associations. A) Pb phosphate rimming
cerussite and B) galena with iron oxide (no lead) rimmed
by Pb phosphate.
PHOTO 14. Backscatter photomicrograph of MnPb oxide cementing
silicates from sample RW001-250.
PHOTO 15. Photomicrographs from sample FH001-250 illustrating A)
galena rimmed by cerussite and B) MnPb oxide to:FePb
oxide all rimmed. by silicate particles.
a
PHOTO 16. Photomicrograph from sample FH001-250 of complex
cerussite, FePb oxide and FePb sulfate associations.
PHOTO 17. Backsoatter photomicrographs from sample FW007-250.,
showing increased surface areas of cerussite and FePb
sulfate..
s
APPENDIS I
a
1
t
1) Prepare a list o all sample n,_rmh~_r-s
Crean and dryrequirednurr,bc-r of 4ilrn canister=, {moldsi.
7 Labcl .each mold r•,ith its correspondingsample number.
Sha4::e eachsample {decompact_=.ar-,d mires) and pour a +ew grams
into its proper- mold.. DouL-le chec4: to he sr_rre that the sample
n~rnrbers on the mold a.hd the origiinal sa,7,ple match! F:ePlace the
original samples cap at~once to a,voidar_cident~l spillage or
contamination. -
F'lace molds with contained sample into the drying oven for at
least one ho~_rr at approx.. Sri's.
b) Mi;: castinq epo::y according to mant.rfactures directions -For an
riven cure.
F'lace enoughepo>iy i.ntgeach mold to iust cover thegrains_ -
8') Usea stirrinq rod tb blend epo;:y and grains so as to coat all
grains with epo;;y. Four additional epa;:y along the stirring rod.
torinse anyclinginq grainsb acF:.intothemold. The samples
should be covered to a depth of 1/4 to :~/B in.. Make darn sure
the stirring rod is clean before moving nn to the ne::t sample.
Usepaper towels if Necessary to wipe the rod. -
9)Set the mil ds tocureat room temperature in an out of tire. way
place.TNe c-po;:y will generate heatdr_rring thecuring process and
if placed in the oven, theadditional heat will cause the epo::y
to boil_
10) [one at a time {so as net to'confu=_e samples and their id
numbers) remo4e each =_ample from its moldandgrind a flat on the
bact: si-de of itsEpo:;y~castinq. Flipthesample q•der andgrind a
similar flat on the sample portipn of tt,E_ casting, e::posing as
much of the sample as possible. Use a scribe or permanent ink pen
to transfer the `sample number from the mold to the casting.
Repeat the abo~.~e until all castings are processed.
11? Use 600 grit carborund,.~m and a glass pla{=e to fine q_rind the
sample face of E>a Ch car:ti nq
I?) Use 600 grit. wetldry abrasi'_~e o~=,per., stretched. across 'a glass
plate to begin the polishi.nq steps.
13) Continue the polishing with 15 micron diamond on a cloth pad
i:;ed to a steel lap.
14) hle;: t rase b mi crgn diamond or-, a si ,T~i 1 ar 1 ap
1,-;) f-'repolish with 1 micron diamond on another cloth lap. This
step can be sl::iped roost of the time. Man•/ tough r, polish
materials like pYri{:. c- requi re this str_p_
l o? Fbl i sh tt~~c•mpl es with i~_°, ,r;i crop alumina i n a water suspen-
lion on .?. felt.pad fi;:ed to a steel lap.
Ploteso - usF• low sper-d on the polishing laps to a~•~eid "pluck:inq"
of thr-_ samplr.: grains. - coat the surface of the casting with ~.
thin layer of epor,y before beginning the polishing steps if
working 411tti fragile or- uncooperative samples. - utmost care is
required to t~rret•.•c_r'ir_ the losing or crossing of sample numbers.
OOESTIONS? CALL80U-238 5355 i0L1 FREE.
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SIGNATURE RELEASE UNAVAILABLE
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SHIPPER'S CEfl'YjFICATION FOR RESTRICTED AF,Tirr~E~; DA.NCERO -c rr_y
CRECK ONE- T+~7~. 49 CFR ^ IATA/ICAO (TYPE OR PRINT)
UN.OR ~~- WAMITY AND PACKING AUTHOR-
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THIS SHIPMENTiS WITHIN THE- ~ PASSENGER 0 (OEIETE-NONAPPLICABUi)
TPPNSPORT ' ~ ®~. AIRCPAFT ,..~`- _-, .:/
pETAIL$ .LIMITATIONS PRESCRIBED FOfi.
AIRPORT OF DEPARTURE AIRPORT OF DESTINATION SHIPMENT ® NON-RADIOACTNE / (DELETE-NONAPPLICABLE)
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IF ACCEPTABLE FOR PASSENGER AIRCRAFT,. THIS SHIPMENT CONTAINS RADIOACTIVE MATERIAL INTENDED FOR USE IN, OR INCIDENT
T0, RESEARCH, MEDICAL DIAGNOSIS ORTREATMENT.
NAME AND ARE CLASS FLED, P COKED, MAROKEDAND LABELED, DAAREFN ALL RESPECTSaINEPROPER CONDITION FORYTRANSPO T BY LAIR
ACCORDING TO THE APPLICABLE INTERNATIONAL AND NATIONAL GOVERNMENT REGULATIONS.
PLACE,PND DATE
NAME AND TITLE OF SHIPPER ~-. ~- ~ -
sIGNAfiuHE oP SHIPPER ~
SEE WARNIK
i'EME NC(T PHONE NUMBER ~ ON BACK