RCRA SW-846 METHODS FOR DETERMINING CHLORINE AND OTHER HALOGENS IN USED OIL

Method Title Description of Procedure Analytes Detected Sensitivity (ppm) Notes

8021B Halogenated Volatile Purge-and-trap (or dilute and shoot Applicable to EQLs of 0.040 to Method does not
Organics by for oils) gas chromatography (GC) individual volatile 0.625 mg/L in non- provide a total
GC/HECD: Capillary procedure using a Hall Electrolytic organic compounds water miscible waste. chloride number.
Column Technique Conductivity Detector (HECD). in oil by dilute and Very low detection The HECD is a
shoot sample limit. relatively low-cost
introduction. GC detector
when compared
to the MS.

8260B Volatile Organic Purge-and-trap (or dilute and shoot Applicable to EQLs of about 2.5 Method does not
Compounds by for oils) gas chromatography (GC) individual volatile mg/L in non-water provide a total
GC/MS: Capillary procedure using a mass organic compounds miscible waste. Very chloride number.
Column Technique spectrometer (MS) detector. in oil by dilute and low detection limit. The MS detector
shoot sample is an expensive,
introduction. complex
detector.

9020B Total Organic A sample of water is passed Applicable to all MDL of 0.005 mg/L Generates a
Halides (TOX) through a column of activated organic halides for drinking water and single total halide
carbon, the column is washed to except fluorine in ground waters. number. Method
remove inorganic halides, the drinking water or is not
remaining halides are combusted, ground waters that do applicable to
and detected with a not contain an amount oil matrices.
microcoulometric detector. of inorganic halides in
excess of 20,000
times.

5050 Bomb Combustion A sample of oil is oxidized by This procedure does Not applicable. This Applicable to
Method for Solid combustion for 30-40 minutes in a not detect halides or is not a solid waste, oils,
Waste bomb containing oxygen under halogenated determinative fuels, and related
pressure. The resulting combustate compounds. Rather, procedure. materials.
is analyzed by Methods 9056, this procedure
9252A, or 9253. prepares oil samples
for analysis by other
determinative
methods.

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 RCRA SW-846 METHODS FOR DETERMINING CHLORINE AND OTHER HALOGENS IN USED OIL

Method Title Description of Procedure Analytes Detected Sensitivity (ppm) Notes

9056 Anion For oils, 2-3 mL of combustate from This procedure can Minimum DL of 0.05 The only method
Chromatography Method 5050 is injected into an ion sequentially determine mg/L for F- and 0.1 that can be used
Method chromatograph and is pumped chloride, fluoride, mg/L for Br-, Cl-, and to determine the
through 3 different ion exchange bromide, nitrate, nitrite, the other ions. Very conc. of each
columns with halogens detected by phosphate, and sulfate low detection limit. halide group (F-,
a conductivity detector. in combustate. Cl-, or Br-).

9253 Chloride (Titrimetric, For oils, combustate from Method This method can This method is Bromide, iodide,
Silver Nitrate) 5050 is adjusted to pH 8.3 and is determine chloride from intended for oxygen and sulfide are
titrated with silver nitrate solution in bomb combustate. bomb combustates also titrated.
the presence of potassium Bromide, iodide, and and waters where the Ortho- and
chromate indicator. sulfide are titrated chloride content is 5 polyphosphate
along with the mg/L or more. can interfere at
chloride. concentrations
above 250 and 25
mg/L,
respectively.

9075 Test Method for Total A well mixed sample is loaded into This method can The applicable range This method
Chlorine in New and an X-ray fluorescence (XRF) determine the total of this method is from does determine
Used Petroleum spectrometer. The intensities of the chlorine in new and 200 mg/kg to percent total chloride
Products by XRF chlorine K alpha and sulfur K alpha used oils, fuels, and levels of chlorine in concentration.
Spectrometry lines are measured using a related materials. oil matrices. One sample from
calibrated system. The sulfur Possible interferants each group of
intensity is used to correct for include metals, water, closely related
absorption by sulfur. Free water is and sediments in the samples should
a major interferant and should be oil. Spike recovery be spiked to
removed before analysis. measurements on used confirm that
crankcase oil showed matrix effects are
that diluting samples 5 not significant.
to 1 allowed accurate
measurement on 80%
of the samples.

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 RCRA SW-846 METHODS FOR DETERMINING CHLORINE AND OTHER HALOGENS IN USED OIL

Method Title Description of Procedure Analytes Detected Sensitivity (ppm) Notes

9076 Test Method for Total A sample is placed in a quartz boat This method can The applicable range This method
Chlorine in New and at the inlet of a high-temperature determine total chlorine of this method is from does determine
Used Petroleum quartz combustion tube. An inert in new and used oils, 10 to 10,000 mg/kg total chloride
Products by carrier gas sweeps across the inlet fuels, and related of chlorine in oil concentration
Oxidative while oxygen flows to the center of materials. Bromine matrices. along with some
Combustion and the combustion tube. The boat and and iodine will also of the bromide
Microcoulometry sample are passed through a give a positive and iodide
temperature zone of about 300EC to response. However, concentration
volatilize the light ends. The sample because oxyhalides of present.
is then advanced to the center of the bromine and iodine do
combustion tube, which is at not react in the titration
1000EC, where the chlorine is cell, only about a 50%
converted to chloride and microequivalent
oxychlorides, which then flow into response is detected
an attached titration cell where they from them.
quantitatively react with silver ions.
The total current required to
coulometrically replace the silver
ions is a measure of the chlorine
present in the sample.

9077 Test Method for Total Method A: The CHLOR-D-TECT This method can This method is semi- This method can
Chlorine in New and 1000 by Dexsil Corporation, involves determine whether or quantitative. Results determine total
Used Petroleum dispersing a sample of oil (about 0.4 not a sample contains are reported as being halogens as
Products (3 Different g by volume) in a solvent and greater than or less above or below 1000 chloride. Each
Field Test Kit reacting with a mixture of metallic than 1000 ppm of total mg/kg of chlorine sample should be
Methods) sodium catalyzed with naphthalene chloride in new and (along with bromide tested twice. If
and diglyme at ambient used oils, fuels and and iodide) in oil the results do not
temperature. All halides in the related materials. matrices. agree then a third
mixture are extracted into an Fluoride, bromide, test must be
aqueous buffered solution and and iodide are also performed.
titrated with mercuric nitrate using a titrated and reported
diphenyl-carbazone indicator to a as chloride in the
blue-violet endpoint. procedure.

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 RCRA SW-846 METHODS FOR DETERMINING CHLORINE AND OTHER HALOGENS IN USED OIL

Method Title Description of Procedure Analytes Detected Sensitivity (ppm) Notes

9077 Method B: The Quanti-Chlor Kit This method can The applicable range This method can
(cont.) from Chemetrics Inc., involves a determine total chlorine of this method is 750 determine total
reverse titration of a fixed volume of in new and used oils, to 7000 mg/kg halogens as
mercuric nitrate with the extracted fuels, and related chlorine in oil chloride. Each
sample to an endpoint that is materials. Fluoride, matrices. sample should be
denoted by a change from blue to bromide, and iodide tested twice. If
yellow in the titration vessel. are also titrated and the results do not
reported as chloride agree within 10%
in the procedure. RPD a third test
should be run.

Method C: The CHLOR-D-TECT This method can The applicable range This method can
Q4000 from Dexsil Corporation determine total chlorine of this method is 300 determine total
involves a titration of the extracted in new and used oils, to 4000 mg/kg of halogens as
sample with mercuric nitrate by fuels, and related chlorine in oil chloride. Each
means of a 1- mL microburette to an materials. Fluoride, matrices. sample should be
endpoint that is denoted by a bromide, and iodide tested twice. If
change from pale yellow to red are also titrated and the results do not
violet. The concentration of chlorine reported as chloride agree within 10%
in the original oil is then read from a in the procedure. RPD, a third test
scale on the microburette. should be run.