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SEMI C36-0705 © SEMI 1981, 2005 4 Area B 1 = Peak Area o f Ion from Instrument (H 2 O) Blank Area Std 1 = Peak Area of Ion from Spiked Standard Area B 2 = Peak Area o f Ion from Standard Blank Conc. Of Std 1 = Concentrat…
SEMI C36-0705 © SEMI 1981, 2005 3
Dilute both cups to 10.0 g using water meeting the criteria for Type E1.1 in ASTM D5127. Mix. Prepare reagent
blank.
8.5.2.3 Analysis — Using the solutions from ¶8.5.2.2 and reagent blank, analyze elements specified by graphite
furnace atomic absorption spectroscopy using manufacturer’s recommended procedure.
8.5.3 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), calcium (Ca), copper (Cu), iron (Fe), lithium (Li),
magnesium (Mg), manganese (Mn), 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’.
8.5.3.1 Sample Preparation — In a clean environment, weigh 5.00 g of sample into each of two 30 mL
polypropylene cups. To one of the cups make standard addition. Add 5.00 g of water meeting the criteria for
Type E1.1 in ASTM D5127 to each cup. Mix.
8.5.3.2 Analysis — Using the solutions from ¶8.5.3.1 and reagent blank, analyze elements specified by plasma
emission spectroscopy using manufacturer’s recommended procedure.
8.6 Trace Anion Analysis
8.6.1 Ion chromatography has been used successfully for the determination of anion impurities at the values
specified for each of the following: chloride (Cl), nitrate (NO
3
) and sulfate (SO
4
). Alternative methods may be used
as long as they are validated for each anion according to SEMI C1, ‘Method Validation’.
8.6.2 The ion chromatography columns
2
used were as follows: ASRS-ULTRA Suppressor (2 mm), IonPac AS6-
ICE Pre-separator (9 mm), IonPac AG11-HC Concentrator (4 mm), IonPac AG11-HC Guard (2 mm), IonPac
AS11-HC Analytical (2 mm), IonPac ATC-1 Anion Trap Column (2 mm). Configure the ion chromatography
system as described in references
3,4
. Eluent may be NaOH or generated KOH using EG40 Eluent Generator
2
.
8.6.3 The following ion chromatography conditions were used:
Eluent 20 mM KOH or NaOH isocratic for 30 min, stepped to 100 mM for 10 min, return
to 20 mM for 5 min
Eluent Flow Rate 0.38 mL/min
Pre-separation Flow Rate 0.5 mL/min
Pre-separation time 8 min
Concentrator collection time 4 min
Sample Volume
200 L
Detection Suppressed Conductivity
Suppressor ASRS, Auto-suppression Recycle Mode
Current Setting 50 mA
Sample dilution 1:1 with de-ionized water (high purity)
Standard High purity phosphoric acid spiked with 1 ppm Cl, 12 ppm SO
4
and 5 ppm NO
3
8.6.4 Calculation of Results
Ion Concentration =
(Area S
1
– Area B
1
) (Conc. Of Std
1
) (Dilution Factor)
Area Std
1
– Area B
2
Area S
1
= Peak Area of Sample Ion
2 Available from Dionex, Sunnyvale, CA, (
www.dionex.com)
3 “Automated trace anion determinations in concentrated electronic grade phosphoric acid by ion chromatography”, F. S. Stover, J. Chromatogr.
A, 956 (2002) 121-128.
4 “The determination of trace anions in concentrated phosphoric acid”, Dionex Technical Note 44, Dionex, Sunnyvale, CA, 1998.
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.