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SEMI C30-1101 © SEMI 1978, 2001 HYDRO GEN PEROXIDE 4 specified f or each of the following metals: aluminum (Al), antim ony (Sb), arsen ic (As), barium (Ba), beryl l ium (Be), bism uth (Bi), boron (B ), calcium (Ca), chro…

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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.
HYDROGEN PEROXIDE SEMI C30-1101 © SEMI 1978, 20015
10.3.2 Special Reagents
10.3.2.1 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.
10.3.2.2 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.
10.3.2.3 Potassium Carbonate Solution — Prepare a
solution containing 500 mg of reagent grade potassium
carbonate (K
2
CO
3
) in 100 mL of water meeting the
criteria for Type E1.1 in ASTM D 5127.
10.3.3 Sample Preparation
10.3.3.1 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 8: For safety purposes, a decomposition aid such as a
platinum strip should be used.
10.3.4 Analysis
10.3.4.1 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.
10.3.4.2 Columns — Precolumn should be AG4-A
(Dionex) or equivalent, and separation column should
be AS4-A (Dionex) or equivalent.
10.4 Trace Metals Analysis
10.4.1 The following method has given satisfactory
results in determining metal ion impurities at the values
specified for each of the following metals: aluminum
(Al), antimony (Sb), arsenic (As), boron (B), cadmium
(Cd), calcium (Ca), chromium (Cr), cobalt (Co), copper
(Cu), gold (Au), iron (Fe), lead (Pb), lithium (Li),
magnesium (Mg), manganese (Mn), molybdenum (Mo),
nickel (Ni), potassium (K), silver (Ag), sodium (Na),
strontium (Sr), tin (Sn), titanium (Ti), vanadium (V),
and zinc (Zn). 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.
10.4.2 Special Reagents
10.4.2.1 Nitric Acid, Ultra Pure — Use nitric acid
specified for low metal ion content.
10.4.2.2 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.
10.4.2.3 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.
10.4.2.4 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.
10.4.3 Sample Preparation
10.4.3.1 In a clean environment, place 20 g of sample
into a tared FEP bottle and add 20 µL of the indium
internal standard.
10.4.4 Analysis
10.4.4.1 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.
11 Grade 4 Procedures
NOTE 9: 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 10: Each laboratory is responsible for verifying the
validity of each method within its own operation.
11.1 Non-Metal Impurities
11.1.1 See Section 8, which contains procedures for the
following tests:
Assay
11.2 TOC
11.2.1 Equipment
11.2.1.1 TOC analyzer capable of analyzing total
oxidizable carbon in 31% H
2
O
2
. Validated
instrumentation includes TOC analyzer using a high
temperature platinum catalyst.
11.2.2 Special Reagents
11.2.2.1 Water — The water used for all of the
dilutions, calibrations, and standards should be the