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3500-Mn A. Introduction
1. General Discussion Samples that have been exposed to air may give low results
due to precipitation of manganese dioxide (MnO2). Add 1 drop
a. Principle: Persulfate oxidation of soluble manganous com- 30% hydrogen peroxide (H2O2) to the sample, after adding the
pounds to form permanganate is carried out in the presence of special reagent, to redissolve precipitated manganese.
silver nitrate. The resulting color is stable for at least 24 h if c. Minimum detectable concentration: The molar absorptivity
excess persulfate is present and organic matter is absent. of permanganate ion is about 2300 L g⫺1 cm⫺1. This corre-
b. Interference: As much as 0.1 g chloride (Cl⫺) in a 50-mL sponds to a minimum detectable concentration (98% transmit-
sample can be prevented from interfering by adding 1 g mercuric tance) of 210 g Mn/L when a 1-cm cell is used or 42 g Mn/L
sulfate (HgSO4) to form slightly dissociated complexes. Bro- when a 5-cm cell is used.
mide and iodide still will interfere and only trace amounts may d. Quality control (QC): The QC practices considered to be
be present. The persulfate procedure can be used for potable an integral part of each method can be found in Section 3020.
water with trace to small amounts of organic matter if the period
2. Apparatus
of heating is increased after more persulfate has been added.
For wastewaters containing organic matter, use preliminary
Colorimetric equipment: One of the following is required:
digestion with nitric and sulfuric acids (HNO3 and H2SO4) (see
a. Spectrophotometer, for use at 525 nm, providing a light
Section 3030G). If large amounts of Cl⫺ also are present, boiling path of 1 cm or longer.
with HNO3 helps remove it. Interfering traces of Cl⫺ are elim- b. Filter photometer, providing a light path of 1 cm or longer
inated by HgSO4 in the special reagent. and equipped with a green filter having maximum transmittance
Colored solutions from other inorganic ions are compensated near 525 nm.
for in the final colorimetric step. c. Nessler tubes, matched, 100-mL, tall form.
https://doi.org/10.2105/SMWW.2882.059 1
MANGANESE (3500-Mn)/Persulfate Method
a. Treatment of sample: If a digested sample has been prepared g Mn (in 100 mL final volume)
mg Mn/L ⫽
according to directions for reducing organic matter and/or excessive mL sample
https://doi.org/10.2105/SMWW.2882.059 2
MANGANESE (3500-Mn)/Persulfate Method
A synthetic sample containing 120 g Mn/L, 500 g Al/L, RICHARDS, M.D. 1930. Colorimetric determination of manganese in
50 g Cd/L, 110 g Cr/L, 470 g Cu/L, 300 g Fe/L, 70 g biological material. Analyst 55:554.
Pb/L, 150 g Ag/L, and 650 g Zn/L in distilled water was NYDAHL, F. 1949. Determination of manganese by the persulfate method.
analyzed in 33 laboratories by the persulfate method, with a Anal. Chem. Acta. 3:144.
relative standard deviation of 26.3% and a relative error of 0%. MILLS, S.M. 1950. Elusive manganese. Water Sewage Works 97:92.
A second synthetic sample, similar in all respects except for SANDELL, E.B. 1959. Colorimetric Determination of Traces of Metals,
50 g Mn/L and 1000 g Cu/L, was analyzed in 17 laboratories 3rd ed. Chapter 26. Interscience Publishers, New York, N.Y.
by the persulfate method, with a relative standard deviation of DELFINO, J.J. & G.F. LEE. 1969. Colorimetric determination of manga-
50.3% and a relative error of 7.2%. nese in lake waters. Environ. Sci. Technol. 3:761.
https://doi.org/10.2105/SMWW.2882.059 3