YELLOW RAIN-ANALYSIS EVALUATION OF WATER SAMPLES
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00037499
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December 28, 2022
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September 26, 2017
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Case Number:
F-2012-01432
Publication Date:
September 26, 1984
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Analytical Research Division
Research Directorate
26 September 1984
Analysis/Evaluation of Water Samples
A shipment designated 10027X(4) was received by the Analytical Research
Division. 10 February 1984, from FSIC. The shipment consisted of seven water
samples. One sample, designated 10027X(4)-1, identified with CB840119-1XX,
consisted of approximately 3 oz. of water containerized in a narrow neck screw
top amber bottle (figure 1). It was taken from a well which had reportedly
been poisoned. The second sample, designated 100214(4)-2. identified with
CB840119-2XX, consisted of approximately 3 oz. of water containerized in a
narrow neck screw top amber bottle (figure 1). It was taken from a second well
which had also reportedly been poisoned. The third sample, designated 10027X(4)-3.
Identified with C8840130-1DI, consisted of approximately 4 oz. of water con-
tainerized in a wide mouth screw top jar (figure 1). This sample was drawn from
the same well as 10027X(4)-1 after it had been emptied and put back in use. The
fourth sample, designated 10027X(4)-4. identified with C8840130-20L, consisted
of approximately 4 oz. of water containerized in -a wide mouth screw top jar
(figure 1). This sample was drawn from the same well as 10027X(4)-2 after it
had been emptied and put back in use. The other three samples, designated
10027X(4)-5, 10027X(4)-6 and 10027X(4)-7, identified with C8840130-301, C8840130-4DL
and CB840130-501, were reportedly reference samples from nearby wells. Each
Consisted of approximately 4 oz. of water containerized in a wide mouth screw top
jar (figure 1). Due to lack of cushioning, sample 10027X(4)-6 was brcken in
transit. Approximately 2 ml of the sample was recovered intact and containerized
In a glass screw top vial at CRDC. An empty jar was inchded in the shipment as
a reference blank.
Vapor samples withdrawn from within each sample enclosure were subjected to
analysis by gas chromatography/mass spectrometry (GC/MS). A portion of each
sample was subjected to purge and trap (sparge) MS analysis. Neat samples Were
analyzed by ion chromatography (IC), thin layer chromatography (TLC), MS for
trichothecenes and for determination of pH. Portions of each sample were
extracted with chloroform. The extracts were analyzed by TLC and infrared
spectrometry (IR).
10027X(4)-1 (CB840119-1flt) well I water, poisoned
The GC/MS spectra of the vapor associated with the water identified the
presence of traces of phenol. Neither the spa rge technique nor the chloroform
extract gave a definitive GC/MS spectra. The pH was determined to be 6.5.
IC detected 1 ppm fluoride, with no other ions present. No detectable components
were separated on either the neat water or the chloroform extract by TLC.
Derivatization with negative ion chemical ionization MS detection was negative
for trichothecenes. IR spectra identified the presence of trace quantities of
aliphatic hydrocarbons and possibly KNO3.
Classified CIA
Declassify: OADR
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10027X(4)-2 (CB840119-2XX) well 2 water, poisoned
The GC/NS spectra of the vapor associated With the water identified the
presence of traces of phenol. Neither the sparge technique nor the chloroform
extract gave a definitive GC/M5 spectra. The pH was determined to be 6.0.
IC detected 0.1 ppm fluoride, with no other ions detected. No detectable
components were separated from either the neat water or the chloroform extract
by TLC. Derivatization with negative ion chemical ionization MS detection
was negative for trichothecenes. IR spectra identified the presence of trace
quantities of hydrocarbons, possibly silicates as soil and possibly (NH4)2CO3.
10027X(4)-3 (CR840130-1E0 well'f water, after cleanup
Neither the vapor associated with the water nor the sparge technique nor
the chloroform extract gave a definitive GC/MS spectra. The pH was determined
to be 6.5. IC detected 0.2 ppm fluoride, with no other ions detected.
No detectable components were separated by TLC. Derivatization with negative
ion chemical ionization MS detection was negative for trichothecenes. IR
spectra identified the presence of aliphatic hydrocarbons and the possible
presence of Si02 probably as soil.
10027X(4)-4 (CB840130-201) well 2 water, after cleanup
The GC/MS spectra of the vapor associated with the water identified traces
of phenol. Neither the sparge technique nor the chloroform solubles gave a
definitive GC/MS spectra. The pH was determined to be 6.5. =IC detected
0.2 ppm fluoride, with no other ions detected. No detectable components were
separated by TLC. Derivatization with negative ion chemical ionization MS
detection was negative for trichothecenes. IR spectra identified the presence
of traces of aliphatic hydrocarbons and possible traces of soil and phosphate.
10027X(4)-5 (C8840130-300 water from reference well
The GC/M5 spectra of the vapor associated with the water identified the
presence of traces of phenol. The sparge technique gave no definitive GC/MS
spectra. Analysis of the chloroform solubles by GC/MS showed only one possible,
unidentified component Mu = 202. The pH was determined to be 6.5. -IC
detected 0.2 ppm fluoride, with no other ions detected. No detectable components
were separated by TLC. Derivatization with negative ion chemical ionization
MS detection was negative for trichothecenes. IR spectra detected only a
trace of aliphatic hydrocarbon.
10027X(4)-6 (C8840130-400 water from reference well
This sample was broken in transit. Only vapor sampling and TLC were per-
formed on the recovered water. The analysis data may be due to exposure to
packaging contents or be real. The GC/MS spectra of the vapors associated
with the water identified the presence of a trace of diphenyl amine. No
detectable components were separated by TLC.
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10027X(4)-7 (CB840130-500 water from reference well
The GC/MS spectra of the vapor associated with the water identified the
presence of a trace of phenol. The sooty technique detected SO2 and an
aliphatic hydrocarbon. The chloroform solubles gave no definitive GC/MS
spectra. IC detected 0.1 ppm fluoride, with no other ions detected. No
detectable components were separated by TLC. Derivatization with negative
Ion chemical ionization MS detection was negative for trichothecenes. IR
spectra identified the presence,of aliphatic hydrocarbons and possibly soil.
Conclusion
No evidence of any known CW agents, writ degradation products or
trichothecenes was detected. The suspect water contained little or nothing
beyond the components of the reference water. -The 1 ppm fluoride detected
in the first 'contaminated" sample is far below a hazardous level. Each of
the samples were very slightly acid which is also normal. The suspect samples
appear to be innocuous. This does not preclude the possibility of a contaminant
having been present at one time and lost through volatilization or dilution
prior to sampling.
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