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SEMI C36-0705 © SEMI 1981, 2005 5 9.4.4 Analysis 9.4.4.1 Using the prepared sample, anal yze the sulfur content usin g inductively c oupled plasma (ICP) spectros copy that has been standardize d using appropriate sulfur …

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SEMI C36-0705 © SEMI 1981, 2005 4
Area B
1
= Peak Area of Ion from Instrument (H
2
O) Blank
Area Std
1
= Peak Area of Ion from Spiked Standard
Area B
2
= Peak Area of Ion from Standard Blank
Conc. Of Std
1
= Concentration of Ion in Spiked Standard
9 Grade 2 Procedures
9.1 Assay — Weigh to the nearest 1 mg about 1 mL of sample in a 250 mL glass-stoppered flask, dilute with 120
mL of water, add 0.5 mL of thymolphthalein indicator solution, and titrate with standardized 1 N sodium hydroxide
to the first appearance of a blue color against a white background.
% Assay =
mL
N
of NaOH
4.900
Weight of sample(g)
9.2 Chloride — Dilute 9 mL (15 g) of sample with 25 mL of water, and add 0.5 mL of nitric acid and 1 mL of silver
nitrate reagent solution. Any turbidity produced should be no greater than that produced when 0.015 mg of chloride
ion (Cl) is treated as the sample.
9.3 Nitrate — Prepare the following solutions:
Sample Solution A: Add 3 mL (5 g) of sample to 2mL of water.
Dilute to 50 mL with brucine sulfate reagent
solution, and mix.
Control Solution B: Add 3 mL (5 g) of sample to 0.025 mg of nitrate
ion (NO
3
). Dilute to 50 mL with brucine sulfate
reagent solution, and mix.
Blank Solution C: Use 50 mL of the brucine sulfate reagent
solution.
9.3.1 Heat the three solutions in a preheated (boiling water) bath for 10 minutes. Cool rapidly in an ice bath to
room temperature. Set a spectrophotometer at 410 nm and, using 1 cm cells, adjust the instrument to read zero
absorbance with Blank Solution C in the light path. Then determine the absorbance of Sample Solution A. Adjust
the instrument to read zero absorbance with Sample Solution A in the light path and determine the absorbance of
Control Solution B. The absorbance of Sample Solution A should not exceed that of Control Solution B.
9.4 Sulfate
9.4.1 The following inductively coupled plasma (ICP) method has given satisfactory results for the determination of
sulfate (SO
4
) by the analysis of sulfur (S) and subsequent calculation to determine the stoichiometric equivalent of
sulfate.
NOTE 3: While this method has been shown to accurately determine sulfate concentration in phosphoric acid, the ICP
methodology actually evaluates sulfur. Therefore, other sulfur species (organic, etc.) will also be determined by this method, and
the “calculated” sulfate value may be higher than the actual sulfate concentration in a given sample.
9.4.2 Special Reagents
9.4.2.1 Water — The water used for all dilution, calibration, and standards should meet, at a minimum, the criteria
for Type E1.1 in ASTM D5127.
9.4.2.2 Scandium Internal Standard — A scandium standard solution is utilized such that final diluted samples will
have a scandium concentration of 40 ppm.
9.4.3 Sample Preparation
9.4.3.1 Dilute 20 g of phosphoric acid to 100 mL with water. (An aliquot of the concentrated scandium standard
solution should also be added during the dilution process such that the final diluted sample will have a scandium
concentration of 40 ppm.)
SEMI C36-0705 © SEMI 1981, 2005 5
9.4.4 Analysis
9.4.4.1 Using the prepared sample, analyze the sulfur content using inductively coupled plasma (ICP) spectroscopy
that has been standardized using appropriate sulfur standard solutions. A wavelength of 180.731 nm has been
shown to give satisfactory results.
9.4.5 Calculation
9.4.5.1 The associated sulfate (SO
4
) concentration is determined using the stoichiometric conversion (SO
4
= 3 S
9.5 Trace Metal Analysis
9.5.1 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), antimony (Sb), arsenic (As), cadmium (Cd),
calcium (Ca), chromium (Cr), cobalt (Co), copper (Cu), gold (Au), iron (Fe), lead (Pb), lithium (Li), magnesium
(Mg), manganese (Mn), nickel (Ni), potassium (K), sodium (Na), strontium (Sr), titanium (Ti), and zinc (Zn).
Alternate methods may be used as long as they are validated for each trace metal according to SEMI C1, ‘Method
Validation’.
9.5.1.1 Special Reagents
9.5.1.1.1 Phosphoric Acid, Ultra Pure — Use phosphoric acid specified for ultra low metal ion content.
9.5.1.1.2 Nitric Acid, Ultra Pure — Use nitric acid specified for ultra low metal ion content.
9.5.1.1.3 Water — The water used for all dilution, calibration, and standards should meet, at a minimum, the criteria
for Type E1.1 in ASTM D5127.
9.5.1.1.4 Internal Standard Stock Solution — An internal standard stock solution containing beryllium (Be),
germanium (Ge), indium (In), lutetium (Lu), and scandium (Sc) is utilized such that final measured solutions will
have a concentration of 100 ppb of each internal standard element.
9.5.1.1.5 External Standard Stock Solution — An external standard stock solution containing the elements in ¶9.5.1
and the internal standard elements in¶9.5.1.1.4 is utilized such that final diluted external calibration standards will
have appropriate concentrations for sample elements and will contain 100 ppb of internal standard elements.
9.5.2 Sample Preparation — In a clean environment, weigh 4.00 g of sample into a 100 mL polypropylene flask.
Add an aliquot of the internal standard stock solution such that the final diluted sample will have a concentration of
100 ppb of each internal standard element. Add 2 mL of nitric acid, ultra pure, and dilute to 100 mL with Type E1.1
water.
9.5.2.1 Analysis — Analyze elements utilizing inductively coupled plasma mass spectrometry (ICP - MS).
Calibrate the sample elements with matrix matched blank and external standards.
9.6 Trace Anion Analysis — see ¶8.6, which contains procedures for trace anions.
10 Grade 3 Procedures
10.1 Assay — Weigh to the nearest 1 mg about 1 mL of sample in a 250 mL glass-stoppered flask, dilute with 120
mL of water, add 0.5 mL of thymolphthalein indicator solution, and titrate with standardized 1 N sodium hydroxide
to the first appearance of a blue color against a white background.
10.2 Chloride — Dilute 9 mL (15 g) of sample with 25 mL of water, and add 0.5 mL of nitric acid and 1 mL of
silver nitrate reagent solution. Any turbidity produced should be no greater than that produced when 0.015 mg of
chloride ion (Cl) is treated as the sample.
SEMI C36-0705 © SEMI 1981, 2005 6
10.3 Nitrate — Prepare the following solutions:
Sample Solution A: Add 3 mL (5 g) of sample to 2 mL of water.
Dilute to 50 mL with brucine sulfate reagent
solution, and mix.
Control Solution B: Add 3 mL (5 g) of sample to 0.025 mg of
nitrate ion (NO
3
) Dilute to 50 mL with
brucine sulfate reagent solution, and mix.
Blank Solution C: Use 50 mL of the brucine sulfate reagent
solution.
10.3.1 Heat the three solutions in a preheated (boiling water) bath for 10 minutes. Cool rapidly in an ice bath to
room temperature. Set a spectrophotometer at 410 nm and, using 1 cm cells, adjust the instrument to read zero
absorbance with Blank Solution C in the light path. Then determine the absorbance of Sample Solution A. Adjust
the instrument to read zero absorbance with Sample Solution A in the light path and determine the absorbance of
Control Solution B. The absorbance of Sample Solution A should not exceed that of Control Solution B.
10.4 Sulfate
10.4.1 The following inductively coupled plasma (ICP) method has given satisfactory results for the determination
of sulfate (SO
4
) by the analysis of sulfur (S) and subsequent calculation to determine the stoichiometric equivalent
of sulfate.
NOTE 3: While this method has been shown to accurately determine sulfate concentration in phosphoric acid, the ICP method
actually evaluates sulfur. Therefore, other sulfur species (organic, etc.) will also be determined by this method, and the
“calculated” sulfate value may be higher than the actual sulfate concentration in a given sample.
10.4.2 Special Reagents
10.4.2.1 Water — The water used for all dilution, calibration, and standards should meet, at a minimum, the criteria
for Type E1.1 in ASTM D5127.
10.4.2.2 Scandium Internal Standard — A scandium standard solution is utilized such that final diluted samples
will have a scandium concentration of 40 ppm.
10.4.3 Sample Preparation
10.4.3.1 Dilute 20 g of phosphoric acid to 100 mL with water. (An aliquot of the concentrated scandium standard
solution should also be added during the dilution process such that the final diluted sample will have a scandium
concentration of 40 ppm.)
10.4.4 Analysis
10.4.4.1 Using the prepared sample, analyze the sulfur content using inductively coupled plasma (ICP)
spectroscopy that has been standardized using appropriate sulfur standard solutions. A wavelength of 180.731 nm
has been shown to give satisfactory results.
10.4.5 Calculation
10.4.5.1 The associated sulfate (SO
4
) concentration is determined using the stiochiometric conversion
(SO
4
= 3 × S).
10.5 Trace Metal Analysis
10.5.1 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), antimony (Sb), arsenic (As), barium (Ba), boron
(B), cadmium (Cd), calcium (Ca), chromium (Cr), cobalt (Co), copper (Cu), gold (Au), iron (Fe), lead (Pb), lithium
(Li), magnesium (Mg), manganese (Mn), nickel (Ni), potassium (K), silicon (Si), sodium (Na), strontium (Sr),
titanium (Ti), and zinc (Zn). Alternate methods may be used as long as they are validated for each trace metal
according to SEMI C1, ‘Method Validation’.