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Determination
of Chromium Emissions from Decorative and Hard Chromium Electroplating
and Chromium Anodizing Operations (Isokinetic Method) – USEPA
Method 306
USEPA Method 306 is used for the determination of chromium (Cr) emissions
from decorative and hard chrome electroplating facilities, chromium
anodizing operations, and continuous chromium plating operations at
iron and steel facilities.
An emission sample is extracted isokinetically from the source using
an unheated USEPA Method 5 sampling train, with a glass nozzle and
probe liner, but with the filter omitted. The sample time is
at least two hours. The Cr emissions are collected in an alkaline
solution containing 0.1 N sodium hydroxide (NaOH) or 0.1 N sodium
bicarbonate (NaHCO3). The collected samples are recovered using
an alkaline solution and are then transported to the laboratory for
analysis.
Total chromium samples with high chromium concentrations (>35 µg/L)
are analyzed using inductively coupled plasma emission spectrometry
(ICP) at 267.72 nm. The ICP analysis is applicable for this
method only when the solution analyzed has a Cr concentration greater
than or equal to 35 µg/L or five times the method detection
limit.
Alternatively, when lower total chromium concentrations (<35 µg/L)
are encountered, a portion of the alkaline sample solution is digested
with nitric acid and analyzed by graphite furnace atomic absorption
spectroscopy (GFAAS) at 357.9 nm. If it is desirable to determine
hexavalent chromium (Cr+6) emissions, the samples are analyzed using
an ion chromatograph equipped with a post-column reactor (IC/PCR)
and a visible wavelength detector. To increase sensitivity for
trace levels of Cr+6, a preconcentration system is used in conjunction
with the IC/PCR.
Components in the sample matrix causes Cr+6 to convert to trivalent
chromium (Cr+3) or cause Cr+3 to convert to Cr+6. The chromatographic
separation of Cr+6 using ion chromatography reduces the potential
for other metals to interfere with the post column reaction.
For the IC/PCR analysis, only compounds that coelute with Cr+6 and
affect the diphenylcarbazide reaction cause interference. |