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>VGK analytical research and development refort vo. l8lj, December 30, 1970
OTHER LOCATIONS
GENERAL OFFICE
W. G. KRJ.MMRICH PLANT
G. L. Jesses - Annisto .1 T. Eell - Anniston E. G. Wright - Annisto K. W. Dietrich Ji'Q
P. E. Hodges
D. V,'. Jackson R. K. Blowers File
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pEFENDANT^ 1 EXHIBIT^ J
TITLE:
Analysis of Anniston Plant Waste Streams for Metals
PERSONNEL:
L. Briggs, D. Arras, K. Schutzenhofer, K. Webb (H. J. Horner)
PR03LEM:
"Determine levels of metallic elements, cyanide and phenols in plant waste streams.
JUSTIFICATION:
The levels of potentially toxic materials entering the
environment must be known in order to define any problems that
exist in meeting government water quality standards.
SUGARY: A
snslytic^l survsy cf* vssfcs stream samples from
the Anniston Plant- has been completed. The s amples were analyzed
for arsenic, cadmium, chromium, lead, mercury , copper, selenium,
zinc, cyanide and phenols. These are the Pri crity I i II items as
outlined in P. Hodges' memo of Oct. 6.- 1970, "Analysis of Waste
Samples for Metals".
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A brief Ascription of the analytical method used in this work is included in the Detail Section.
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Possible problen areas in meeting the standards for public water
suDolies exist with Lead, Mercury, Selenium and Phenols.
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CONFIDENTIAL
OSw 1069 9.9
This report is ike property of Monsanto Conpcr. y cn:1 th.e re: ip ie r.i is responsible for its safekeeping
oni disposition* it contains conf identic! information of
Copper:/ w.Sicr. must not be
reprcfuctf, revealed tc unauthorized persens or r r ~t outside the company without proper authorization.
This report is to be retained in 0 secure file or destroyed*
WATER_PCB-SD0000051878
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December 30, 1970
Details
A brief description of the analytical methods used in his work follows:
1. Cyanide ( WGK Method A-1003)
This method is based on the FWFCA method from the Nov. 1969 issue of "FwPCA Methods for Chemical Analysis of Water and Wastes'.' Cyanide ion and complex cyanides are converted to hydrocyanic acid (HCN) by reaction in a reflux system of a mineral acid in the presence of magnesium and mercuric ions. The cyanide is absorbed in a solution containing sodium hydroxide. The cyanide ion is then determined colorimetrically using the pyridine pyrozolone reaction.
2. Phenols (WGK Method 12,791)
This is a colorimetric method based on the formation of a color by the reaction of A-aminoantipyrine with phenolic compounds in the presence of an alkaline oxidizing agent. The determination is done automatically with a Tecbnicon Autoanalyzer. This method is calibrated against phenol. The method is non specific and can vary significantly depending on the type of phenolic compounds present.
3. Arsenic (V.'GK Method A-1005)
The sample is digested, if necessary, with sulfuric and nitric acid to destroy organic matter. The arsenic in the sample is reduced to arsine gas which is absorbed in a pyridine solution of silver diethyldithiocarbamate. The resulting red colored complex is measured colorimetrically.
A. Mercury (WGK MethocA-1002)
Samples are treated with KMn04-H2S04 to destroy complexes and
place all mercury in the inorganic form. Mercury salts are
reduced to elemental mercury by stannous chloride and the
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of air. The light absorption by the mercury is measured with
an atomic absorption spectrophotometer.
5. Selenium (iGK Method A-1010)
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Samples r.:o oxidized by an acid-permanganate digestion. Selenaies are then reduced and reacted with 3>3'dianinobenzidine hydi-ucnloride forming a yellow colored complex. The colored complex is extracted with toluene and the color intensity is measured with a soectroohc-tometer.
6. Cadm
(raoaiflcation nf
'd A-1005)
Samples are digested by boiling after edition of nitric and
hydrochloric acid. The pH is adjusts-: is com.plexed by the addition of sodiur
to 6.5 and the cadmium diethyldithiocarbamate.
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December 30, 1970
The complex is extracted vrith methyl iscbutyl ketone and measured by atomic absorpticn spectrophotometry.
7. Copper, Lead, Zinc and Chromium (Modification of V.'C-K Method A-1007)
Samples are digested by boiling after addition of nitric and hydrochloric acid. The pK is adjusted to 4.0 and the metals are ccmplexed by the addition of ammonium pyrollidine . dithiocarbamate. The comple>3sare extracted v.'ith methyl isobutyl ketone and measured by atomic absorption spectrophotometry.
Lab Notebook Ref: I4p44-l4551 14712-14714 14720-14723 13934-13972
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