Document 2RZmrXX8aMeL4d9zeV2VeG89g
Monsanto
10879 80FY/
MONSANTO RESEARCH CORPORATION l DAYTON LABORATORY f DAYTON, OHIO 41407
EASC - PAY ton lOirr/stCTidwi
Analytical r*t o* M*or
sfsonT
HIFONT NO.: MOA-213
RECEIVED
JOt/PROJECT NO.: 404.3200 DATE: 17 July 1941
PERIOD COVERED: TITLE: ANALYSIS OF LANDFILL WELLS
jul" >
.ONSANTC-DAYTON
CENTRAL FILES
AUTHORS:
CM
F. 0. HHainan and R. F. Ivory '
11.
2 1 3 AUTHORS: F . O. H i IOm an a n d K. F . I v o r y
TITLE: A N A LY S IS OF L A N D F II.I. HULLS
ii si
ABSTRACT;
Eight landfill wall water samplas fron the MCI
Kruswrieh plant ware analyzed to determine the preaence or abeence of phenols. PCBs and TCOD. The analytical results are presented in this report.
Technical Approval;
)o^. -Q
Frederick 0. Hileman Senior Research chemiat
Approved byi
i
r>
Robert F. Ivory Environmental Analytical Sciences
Csntsr Service Project Manager
Approval date;
RESTRICTED DISTRIBUTION (see over)
COMPANY CONFIDENTIAL
HONS 220601
DISTRIBUTION
COPY NUMBER
J \. Sullivan 4 D. J. Oahm 5 R. F. I vory 6 J. 0. WiIson * D. 0. Edwards S Central Filet 9 Technical Reports Library
Krununrich
1250 1250 \3A
B2SE 1250,
R2C
ABSTRACT ONLY
R. X. Flitcraf t/Dayton R. M. Scott/1250
Distribution of this report is restricted. Pequeats for
additional copies should be node through the principal
contact at the Monsanto location involved or tha Manager,
Er.vironrer.tal Analytical Sncncei Center, Dayton Laborator-
Dayton, Ohio.
'
acknowledcemest
Contributions of the following Dayton Laboratory personnel to this project ere gratefully acknowledged:
Analysest
F. D. Hilenan
H. M. Strickland A. J. Wright
COMPANY CONFIDENTIAL When no longec needed, or upon request, return this report .to Control Flloo. Dayton.
MONS 220602
ANALYSIS OP LANDFILL WELL WATER SAMPLES FOR TOTAL PHENOLS TETRACI(LOROD1!!ESZO*-OIOx:N AND polyciiloronated biphenyls
Eight (!) water samples were submitted to the Dayton Laboratory for analyses to determine t!.c possible presence and concentra tions of total phenols, polychlorinated biphenyls (PCI) and tctrachlorodibcnio-p-diox ins (TCOD).
Total Phenols
The presence ar.d concentration of phenol in each of the water samples was determined and measured by typical wet chemistry techniques 11], An independent phenol standard was also analyzed i:z quality assurance. The results of these analyses are shown m Table 1.
TABLE 1. ANALYSIS OF LANDFILL WELL NATi? FOR TOTAL PHENOL
well 1 well 2A
well 2> well
well ISA well ns wel 1 2C
no
321
1.290 1.50*
11' 29*
m
^Average cf duplicate analyses.
Reference
standard
ERA 27*7
Otserved value,
O.SC
True value, -SSZit-
0.12
Percent recovery
10S
tlj Standard Methods for Exaninetioa of Hater and wastewater* 14th Edition, Aswrlean Public Health Association,
Washingtoo, DC. 1*74. 11*3 pp.
1
MONS 220403
Polychlorinated Biphenyls (PCB)
500 mb of each water samp1.* and its container were extracted with three (J) SO-mL aliquots of methylene chloride. The combined extracts (sample and container) of each sample were dried and evaporated to 1-mL. Each 1-*L sample was analyzed by a capillary gas chromatography/mass spectrometry (CC/MS) technique. The MS was operated in the Selected Ion Monitor mod* (SIN) to enhance sensitivity and decrease possible interferences. The SIN mod* monitors two ions for each isomer class of PCI's (number of chlorine atoms on the biphenyl molecule). Known PCI standards were analyzed to quantitate sample concentrations. Spikes and duplicates of the samples were run under similar analytical con ditions for quality assurance. Results of these analyses are shown in Table 2.
Tetrachlorodibenzo-p-dioxins (TCOOs)
Eight water samples were received for the analysis of tetrachlorcdibenzo-g-dioxins (TCDO). Two separate 1-liter samples were provided fror. each sit*. On* of the 1-liter bottles for each site was used for the analysis with the other bottle being set aside in the event that soma problem or difficulty occurred in the original analysis. The samples wer* analysed by taking one of the 1-liter bottles and placing S00 mL of the water into each of two 1-liter bottles. One of the $00 mb aliquots was then used for the analysis with the other aliquot used as a replicet* or for spiking with native (unlabeled) 2.3,7.t-TCDO. 200 mL of petroleum ether wee thee added to the original sample bottle end the ooatents wars shaken for 30 seconds to sstrset sny TCOOs
which msy sdhers to the glass. During this time, ell the 500 mb
aliquots were spiked with '*Cu-labeled 2,3.7.1-tcdd and various
$00 mb aliquots wore spiked with native 2,1,7.I-TCDO. 100 mb of
the petroleum ether from the original aampla bottla was then plaqpd into each of tho bottles containing the $00 mb aliquots.
2
HONS 220404
TABLE 2. ANALYSIS OF LANDFILL WELL WATER SAMPLES FOR PCD*
Samele ID
Total
Number of chlorines. uq/L
PCB,
l 2 1 A 5 6 7 tf 9 10 uq/L
well 1
BDL* BDL BOL BDL PDL BOL
BDL DOL BOL BOL
Hell 1 duplicate Hell 2k
M *
*
H* "
M
MM
N
"
well la Hell 2> duplicate
** H
m
Hm
* *
*
** m
well M well *B
le o.s O.S m 3.2 0.7
*
o.s 1.7
**
11.2
BDL
6 6
well ISA well 1S
0.1 BOL BDL " BDL 0.1 **
"
BDL 0.6
M
*t
BOL **
*
well 20
BDL # * *
6
BDL *
m
"
} .9
n.i
0.2 0.6 BDL
aBOL - below detection Unit of D.l uq/L (ppb).
oumtT cowmen, data
Mall B2A spiked with 11> ppb of Aroclor 1354 dot recovery Hell 120 epiked with 111 ppb of Aroclor 1254 61* recovery
mons 220605
Th# bottles were then shaken for five einutea and the water layer removed. The petroleum ether layer was then washed with base followed by sulfuric acid. Column chromatography of the concen trated petroleum ether vkj carried out on a Woelm Basie alumina column collecting the fraction that elutes with the Sot CH,C1,/ Hexane fraction, concentrating to 2$ uL and submitting this aampia for GC/M5 analysis.
The CC/MS analysis was carried out on a Hewlett-Packard 5SISB CC/MS system. The chromatograph was equipped with a J and w 30 meter SE-S4 capillary column. The mass spectrometer was operated in the selected ion monitoring mode following one ion character istic of the labeled TCDD (m/z 334) and three ions characteristic of native TCDD (r,/z 257, 320, 322).
Cuantitation was carried out by ratioinq the response of the native TCDD to the labeled TCDD. The results of the analyses are qiven in Table 3. Sample A15 showed very serious interferences so a different workup of this sample was carried out usinq 100 mL of water at the outeet rather than the 500 mL and alao usinq an initial alumina column clean up step prior to the base end acid washes. The results qiven as *ND* mean none detected at a detection limit qiven in parenthesis. This detection limit depends on the interferences present end sample recovery end thus vsries from sample to sample. The blank is representative of the lower detection limit if there were no interferences. A TCDD was found in the samples from wells 2A and 2B and in the 1,3,5,l-TCDD. The chrometographie traces for the analysis of well 2A is given in Figure 1. The ions being monitored are char acteristic of tike molecular ions of the labeled and unlabeled TCDD end the C0C1 lose for the unlabeled TCDD. Am e point of
reference, the chrometogrephle trees for the 2,3,7,l-TCDD is
givam la Figure 2 showing comparable ions. The quantitation for the 1,3,1,1-TCOO is based on'the celibretion curve generated for this 2,3,7,l-TCDD end may 1m subject to some degree of error.
4
HONS 220*06
TABLE 3. RESULTS FOR THE ANALYSIS Or
TETRACHLORORENKO-g-DIOXINS (TCODa)
Saoi 1 r ID
landfill Well *1
m :*
m * i/a (replieete)
m hi * A9
*9 (pike)
' 99 ' AlS
' AlS (rcpl icit*) ' .MS dplks) * AlS (ipiks)
' 31S * 10
Sl ml
2,1,7,8-TCDO round
ne/L (ppt)
M (<2) KD (<T) TO S) TO (<22) TO XJ5)
4.1
TO X9) TO S) TO S)
11 179 TO 1)
TO X2I
w D
1,1.7.S-TCDD Added
ne/L (ppt)
1.9
19 192
* -
,
Other rcuOe Pound
ne/L loot)
IBS (<10> 89
88
290
4 _4
S)
TO KSl HD KS)
TO 1)
HD Ki> ND (<2)
TO Kl)
*5eriout Interferences prevented the anelyeii of kmnri other than 2,1.7,8TC33 while nair.-aimfMj good sensitivity for I, J. 7,l-TCDO.
An additional connant should also be mads about ths spiking experiments. In sampls 9A9 an interference peak limited ths dstsetion limit to 3.S ppt. When 1.9 ppt of 2.3.7.B-TCDD was spiked into a replicate sampls ths peak grew to 4.B ppt for a difference of 1.3 ppt which is reasonable in view of the uncer tainty in these analyses at these levels. For sample AlS the 5 ppt detection limit was determined by the ultimate sensitivity of the GC/HS and there were no interferences in the second workup of this sample. Therefore the 19 ppt spike should be compared directly to the 13 ppt supl* recovered. Again this result is rtastmBirl s in light of the difficulties encountered in analysing this particular sample.
S HONS 220*07
4
rigux* 1. GC/M8 analyala of Landfill Watar |2A. MQNS 220608
riqur* 2. GC/N9 analyaia of 2,3,7,9-TCDO. HONS 220609