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HYDROGEN PEROXIDE SEMI C30 -1101 © SEMI 1 978, 2001 3 element in t he peroxide matrix. Aqueous acidified standards for tin in 2% hy drochloric acid and other specified elements in 2% n itric acid should be used to determ…

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SEMI C30-1101 © SEMI 1978, 2001 HYDROGEN PEROXIDE2
8.4 TOC
8.4.1 Equipment
8.4.1.1 TOC analyzer capable of analyzing total
organic carbon in water.
8.4.1.2 Platinum sheet 1 × 1 inch, heated in a muffle
oven at 800°C for 15 minutes.
8.4.2 Special Reagents
8.4.2.1 Water — The water used for all of the dilution,
calibration, and standards should meet, at a minimum,
the criteria for Type E1.1 in ASTM D 5127 in regard to
TOC analysis.
8.4.2.2 1000 mg/mL TOC Standard (prepare fresh
weekly) — Weigh accurately 0.2128 g of potassium
acid phthalate into a 100 mL volumetric flask, add
water, shake to dissolve, dilute to volume, and mix
well. Lower standards (prepare fresh daily) can be
made by diluting an aliquot of the 1000 mg/mL to the
appropriate volume.
8.4.3 Sample Preparation — Weigh 50 g of hydrogen
peroxide, to the nearest 0.01 g, into a 400 mL beaker.
Add the platinum sheet to the sample, cover the beaker
with a Teflon watch glass, and allow the reaction to go
overnight (12 hours minimum). Transfer the solution to
a 50 mL volumetric flask, and dilute with water
meeting the criteria for Type E1.1 in ASTM D 5127 to
a final volume of 50 mL.
8.4.4 Analysis — Using the prepared solutions, analyze
TOC by the total organic carbon analyzer after the
instrument has been calibrated with 0, 4, 10, and 20
µg/mL of TOC standards.
8.5 Chloride — Dilute 4.5 mL (5 g) of sample with 15
mL of water. Filter, if necessary, through a chloride-
free filter. Add 1 mL of nitric acid and 1 mL of silver
nitrate reagent solution. Any turbidity produced should
be no greater than that produced when 0.01 mg of
chloride ion (Cl) is treated as the sample.
8.6 Sulfate — To 9 mL (10 g) of sample, add 10 mL of
sodium carbonate reagent solution and evaporate to
dryness in a hood. Dissolve the residue in 10 mL of
water and 1 mL of dilute hydrochloric acid (1 + 19);
filter if necessary. Add 1 mL of barium chloride reagent
solution, mix, and allow to stand for 10 minutes. Any
turbidity developed should be no greater than that
produced when 0.05 mg of sulfate ion (SO
4
) is treated
as the sample.
8.7 Phosphate — Evaporate 4.5 mL (5 g) of sample to
dryness on the steam bath and dissolve the residue in 25
mL of 0.5 N sulfuric acid. Add 1 mL of ammonium
molybdate reagent solution and 1 mL of p-
(methylamino)phenol sulfate reagent solution. Allow to
stand for 2 hours at room temperature. Any blue color
should not exceed that produced in a standard of equal
volume containing 0.01 mg of phosphate ion (PO
4
) and
the quantities of reagents used in the sample.
8.8 Arsenic and Antimony (as As) — To 180 mL (200
g) of sample in a 400 mL beaker, add 5 mL of sulfuric
acid and evaporate to dense fumes of sulfur trioxide in a
hood. Cool, cautiously add 10 mL of water, and again
evaporate to dense fumes of sulfur trioxide. Cool, and
cautiously wash into a generator flask with water to
make a volume of 35 mL. Proceed as described in
General Method for Arsenic (and Antimony) under
SEMI C1, Section 3.4.5, starting with the first sentence
which begins: “Swirl the flask....” Any red color in the
silver diethyldithiocarbamate solution from the sample
should be no greater than that of the standard
containing 0.002 mg of arsenic (As).
8.9 Trace Metal Analysis — The following method has
given satisfactory results in determining trace metal
impurities at the value specified for each of the
following trace metals: aluminum (Al), boron (B),
calcium (Ca), chromium (Cr), copper (Cu), gold (Au),
iron (Fe), lead (Pb), magnesium (Mg), manganese
(Mn), nickel (Ni), potassium (K), sodium (Na), tin (Sn),
titanium (Ti), and zinc (Zn). Alternate methods may be
used as long as appropriate studies demonstrate
recovery between 75–125% of a known sample spike
for half of the value of each specified element.
8.9.1 Special Reagents
8.9.1.1 Nitric Acid, Ultra Pure — Use nitric acid
specified for ultra low metal ion content.
8.9.1.2 Hydrochloric Acid, Ultra Pure — Use
hydrochloric acid specified for ultra low metal ion
content.
8.9.2 Sample Preparation
8.9.2.1 Sodium and Potassium — In a clean
environment, place 10.0 mL of water in a clean
platinum crucible. Slowly add 5.0 mL of hydrogen
peroxide. Allow to stand at room temperature until the
effervescence ceases (approximately 20 minutes).
Swirl. If swirling does not produce any more bubbles,
proceed with analysis. If bubbles remain, allow to stand
for 5 minutes and repeat the swirl until no bubbles are
produced. Run a water blank.
8.9.2.2 Other Elements — Two separate samples of
hydrogen peroxide are acidified to 2% with
hydrochloric acid for the analysis of tin and to 2% with
nitric acid for the analysis of (specified elements).
Standard additions of tin to the matrix acidified with
hydrochloric acid and standard additions of other
specified elements to the matrix acidified with nitric
acid are added to determine the response for each
HYDROGEN PEROXIDE SEMI C30-1101 © SEMI 1978, 20013
element in the peroxide matrix. Aqueous acidified
standards for tin in 2% hydrochloric acid and other
specified elements in 2% nitric acid should be used to
determine instrument responses.
8.9.3 Analysis
8.9.3.1 Using the solution from Section 8.9.2.1,
analyze for specified group 1 elements by flame atomic
absorption spectroscopy. All other elements analyzed
by plasma emission spectroscopy.
9 Grade 2 Procedures
NOTE 4: Each laboratory is responsible for verifying the
validity of the method within its own operation.
9.1 Non-Metal Impurities
9.1.1 See Section 8, which contains procedures for the
following tests:
Assay
Color (APHA)
Free Acid
9.2 TOC
9.2.1 Equipment
9.2.1.1 TOC analyzer capable of analyzing total
organic carbon in water.
9.2.1.2 Platinum sheet 1 × 1 inch, heated in a muffle
oven at 800°C for 15 minutes.
9.2.2 Special Reagents
9.2.2.1 Water — The water used for all of the dilution,
calibration, and standards should meet, at a minimum,
the criteria for Type E1.1 in ASTM D 5127 in regard to
TOC analysis.
9.2.2.2 1000 mg/mL TOC Standard (prepare fresh
weekly) — Weigh accurately 0.2128 g of potassium
acid phthalate into a 100 mL volumetric flask, add
water, shake to dissolve, dilute to volume, and mix
well. Lower standards (prepare fresh daily) can be
made by diluting an aliquot of the 1000 mg/mL to the
appropriate volume.
9.2.3 Sample Preparation
9.2.3.1 Weigh 50 g of hydrogen peroxide, to the
nearest 0.01 g, into a 400 mL beaker. Add the platinum
sheet to the sample, cover the beaker with a Teflon
watch glass, and allow the reaction to go overnight (12
hours minimum). Transfer the solution to a 50 mL
volumetric flask, dilute with water, meeting the criteria
for Type E1.1 in ASTM D 5127, to a final volume of 50
mL.
9.2.4 Analysis
9.2.4.1 Using the prepared solutions, analyze TOC by
the total organic carbon analyzer after the instrument
has been calibrated with 0, 4, 10, and 20 µg/mL of TOC
standards.
9.3 Anions
9.3.1 The following method has given satisfactory
results in determining anion impurities at the values
specified for each of the following anions: chloride
(Cl), phosphate (PO
4
), nitrate (NO
3
), and sulfate (SO
4
).
Alternate methods may be used as long as appropriate
studies demonstrate a recovery between 75–125% of a
known sample spike for half of the value of each
specified anion.
9.3.2 Special Reagents
9.3.2.1 Eluent — Prepare an eluent solution that is 2.2
mM sodium carbonate (Na
2
CO
3
) and 0.75 mM sodium
bicarbonate (NaHCO
3
) in deionized water meeting the
criteria for Type E1.1 in ASTM D 5127. Store eluent
under a helium gas blanket.
9.3.2.2 Regenerant — Prepare a 0.025 N sulfuric acid
(H
2
SO
4
) in deionized water meeting the criteria for
Type E1.1 in ASTM D 5127.
9.3.2.3 Potassium Carbonate Solution — Prepare a
solution containing 500 mg of reagent grade potassium
carbonate (K
2
CO
3
) into 100 mL of water meeting the
criteria for Type E1.1 in ASTM D 5127.
9.3.3 Sample Preparation
9.3.3.1 In a clean environment, place 40 g of sample
into a clean beaker. Add 1 mL of a 5 mg/mL potassium
carbonate solution and evaporate carefully (at 100°C) to
a volume of 0.5 mL. Dilute with water meeting the
criteria for Type E1.1 in ASTM D 5127 to a final
volume of 20 mL.
NOTE 5: For safety purposes, a decomposition aid such as a
platinum strip should be used.
9.3.4 Analysis
9.3.4.1 Using the prepared solutions and blanks,
analyze chloride, nitrate, phosphate, and sulfate by ion
chromatography. Run a reagent blank. Samples and
reagent blanks should be prepared and analyzed in
triplicate.
9.3.4.2 Columns — Precolumn should be AG4-A
(Dionex) or equivalent and Separation column should
be AS4-A (Dionex) or equivalent.
9.4 Trace Metals Analysis
9.4.1 The following method has given satisfactory
results in determining metal ion impurities at the values
SEMI C30-1101 © SEMI 1978, 2001 HYDROGEN PEROXIDE4
specified for each of the following metals: aluminum
(Al), antimony (Sb), arsenic (As), barium (Ba),
beryllium (Be), bismuth (Bi), boron (B), calcium (Ca),
chromium (Cr), cobalt (Co), copper (Cu), gallium (Ga),
germanium (Ge), gold (Au), iron (Fe), lead (Pb),
lithium (Li), magnesium (Mg), manganese (Mn),
molybdenum (Mo), nickel (Ni), niobium (Nb),
potassium (K), silver (Ag), sodium (Na), strontium (Sr),
tantalum (Ta), tin (Sn), titanium (Ti), vanadium (V),
zinc (Zn), and zirconium (Zr). Alternate methods may
be used as long as appropriate studies demonstrate a
recovery between 75–125% of a known sample spike
for half of the value of each specified element.
9.4.2 Special Reagents
9.4.2.1 Nitric Acid, Ultra Pure — Use nitric acid
specified for low metal ion content.
9.4.2.2 1% Nitric Acid Solution — Dilute 10 mL of
ultrapure nitric acid to 1 L of water meeting the criteria
for Type E1.1 in ASTM D 5127.
9.4.2.3 Water — The water used for all the dilution,
calibration, and standards should meet, at a minimum,
the criteria for Type E1.1 in ASTM D 5127 in regard to
cation analysis.
9.4.2.4 Indium Internal Standard — Make up the
indium internal standard solution to a concentration of
20 µg/mL (ppm) from the appropriate concentrated
indium standard solution.
9.4.3 Sample Preparation
9.4.3.1 In a clean environment, place 20 g of sample in
a tared FEP bottle, add 20 µL of the indium internal
standard.
9.4.4 Analysis
9.4.4.1 Using the prepared solutions and blanks,
analyze sodium, potassium, calcium, and iron by
graphite furnace atomic absorption (GFAA) and the
remaining elements by inductively coupled plasma
mass spectrometry (ICP/MS). For calibration, the
standards are made up with the 1% nitric acid solution
and the indium internal standard such that the final
concentration is 20 ng/g of indium. Run a reagent
blank.
10 Grade 3 Procedures
NOTE 6: The analytical procedures associated with this
standard are not intended to be the only acceptable procedure
or the best procedure available. The published procedures
have been found to meet the required criteria for acceptance
of an analytical procedure. Alternate procedures may be used
if they meet the same criteria as the published procedures.
NOTE 7: Each laboratory is responsible for verifying the
validity of each method within its own operation.
10.1 Non-Metal Impurities
10.1.1 See Section 8, which contains procedures for the
following tests:
Assay
Color (APHA)
Free Acid
10.2 TOC
10.2.1 Equipment
10.2.1.1 TOC analyzer capable of analyzing total
organic carbon in water.
10.2.1.2 Platinum sheet 1 × 1 inch, heated in a muffle
oven at 800°C for 15 minutes.
10.2.2 Special Reagents
10.2.2.1 Water — The water used for all of the
dilution, calibration, and standards should meet, at a
minimum, the criteria for Type E1.1 in ASTM D 5127
in regard to TOC analysis.
10.2.2.2 1000 µg/mL TOC Standard (prepare fresh
weekly) — Weigh accurately 0.2128 g of potassium
acid phthalate into a 100 mL volumetric flask, add
water, shake to dissolve, dilute to volume, and mix
well. Lower standards (prepare fresh daily) can be
made by diluting an aliquot of the 1000 µg/mL to the
appropriate volume.
10.2.3 Sample Preparation
10.2.3.1 Weigh 50 g of hydrogen peroxide, to the
nearest 0.01 g, into a 400 mL beaker. Add the platinum
sheet to the sample, cover the beaker with a Teflon
watch glass, and allow the reaction to go overnight (12
hours minimum). Transfer the solution to a 50 mL
volumetric flask, dilute with water, meeting the criteria
for Type E1.1 in ASTM D 5127 to a final volume of 50
mL.
10.2.4 Analysis
10.2.4.1 Using the prepared solutions, analyze TOC by
the total organic carbon analyzer after the instrument
has been calibrated with 0, 4, 10, and 20 µg/mL of TOC
standards.
10.3 Anions
10.3.1 The following method has given satisfactory
results in determining anion impurities at the values
specified for each of the following anions: chloride
(Cl), phosphate (PO
4
), nitrate (NO
3
), and sulfate (SO
4
).
Alternate methods may be used as long as appropriate
studies demonstrate a recovery between 75–125% of a
known sample spike for half of the value of each
specified anion.