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SEMI C41-0705 © SEMI 1978, 2005 5 9 Grade 3 Procedures NOTE 5: Each labo ratory is responsible fo r verifying the validity of the method within its own operation. 9.1 See §7, which contains procedur es fo r the following…

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SEMI C41-0705 © SEMI 1978, 2005 4
8 Grade 2 Procedures
NOTE 3: Each laboratory is responsible for verifying the validity of the method within its own operation.
8.1 Non-Metal Impurities — See §7, which contains procedures for the following tests:
Assay
Water
Color (APHA)
Chloride
Phosphate
Arsenic and Antimony (as As)
Boron
8.2 Trace Metals Analysis
8.2.1 The following method has given satisfactory results in determining trace metal impurities at the values
specified for each of the following metals: aluminum (Al), barium (Ba), beryllium (Be), bismuth (Bi), cadmium
(Cd), 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), thallium (Tl), tin (Sn), titanium (Ti),
vanadium (V), zinc (Zn), and zirconium (Zr). Alternate methods may be used as long as they are validated for each
trace metal according to SEMI C1, ‘Method Validation’.
8.2.2 Special Reagents
8.2.2.1 Nitric Acid, Ultra Pure — Use nitric acid specified for low metal ion content.
8.2.2.2 1% Nitric Acid Solution — Dilute 10 mL of ultrapure nitric acid to 1 L using water meeting the criteria for
Type E1.1 in ASTM D5127.
8.2.2.3 Water — The water used for all the dilution, calibration and standards should meet at a minimum the criteria
for Type E1.1 in ASTM D5127 in regard to trace metal analysis.
8.2.2.4 Indium Internal Standard — Make up an indium internal standard solution to a concentration of 20 mg/mL
(ppm) from an appropriate concentrated indium standard solution.
8.2.2.5 Mannitol Powder — Mannitol powder, reagent grade (ACS)
8.2.2.6 5% Mannitol Solution — Prepare a 5% (by weight), dissolve and dilute 5 g of reagent grade Mannitol
powder (ACS) to 100 g using water meeting the criteria for Type E1.1 in ASTM D5127.
8.2.3 Sample Preparation
8.2.3.1 All Elements — In a clean environment, place 200 g of sample into a PTFE dish. Add 5 mL of the 5%
Mannitol solution and 100 mL of the 1% nitric acid solution. Slowly evaporate on a hot plate to dryness avoiding
loss of sample by effervescence or spattering until 1 to 2 mL remain. Dissolve the residue with 5 mL of the 1% nitric
acid solution by heating on a hot plate at low temperature for several minutes. Cool to room temperature, dilute to
50 mL with 1% nitric acid, add an appropriate concentration of the indium internal standard and mix well. Prepare a
reagent blank.
8.2.4 Analysis
8.2.4.1
Using the prepared solutions and blanks, analyze 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 a suitable concentration of the indium
internal standard.
NOTE 4: Current ICP-MS technology (2004) allows analysis of all trace metals, see Grade 3 Procedures and SEMI C1, ‘ICP-
MS’.
SEMI C41-0705 © SEMI 1978, 2005 5
9 Grade 3 Procedures
NOTE 5: Each laboratory is responsible for verifying the validity of the method within its own operation.
9.1 See §7, which contains procedures for the following tests:
Assay
Color (APHA)
Residue after Evaporation
Water (H
2
O)
9.2 Analysis of Anions
9.2.1 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
), phosphate (PO
4
) and sulfate (SO
4
). Alternate
methods may be used as long as they are validated for each anion according to SEMI C1, ‘Method Validation’.
9.2.2 The ion chromatography columns used were as follows
2
: ASRS-ULTRA Suppressor (2 mm), IonPac AG9-HC
Concentrator (4 mm), IonPac AG9-HC Guard (2 mm), IonPac AS9-HC Analytical (2 mm), IonPac ATC-1 Anion
Trap (4 mm).
9.2.3 The following ion chromatography conditions were used:
Eluent 8.0 mM sodium carbonate/1.5mM sodium hydroxide
Eluent Flow Rate 0.25 mL/min
Rinsing Flow Rate 2.0 mL/min
Sample Volume 5 mL
Detection Suppressed Conductivity
Suppressor ASRS, Autosuppression External Water Mode
Current Setting 100 mA
Sample 2-propanol (high purity)
Anion Spike Level 5 ppb
9.3 Trace Metals Analysis
9.3.1 ICP-MS has been used successfully for the determination of trace metal impurities at the values specified for
each of the following: aluminium (Al), arsenic (As), antimony (Sb), barium (Ba), boron (B), cadmium (Cd), calcium
(Ca), chromium (Cr), coppper (Cu), iron (Fe), lead (Pb), lithium (Li), magnesium (Mg), manganese (Mn), nickel
(Ni), potassium (K), sodium (Na), tin (Sn), titanium (Ti), Vanadium (V) and zinc (Zn). Alternate methods may be
used as long as method validation according to SEMI C1 can be demonstrated.
9.3.2 Special Reagents
9.3.2.1 Nitric Acid, Ultrapure — Use nitric acid specified for low metal content.
9.3.2.2 Water — The water used for all dilution, calibration and standards should meet, at a minimum, the criteria
for Type E1.2 in ASTM D5127 in regard to trace metal analysis.
9.3.2.3 1% Nitric Acid Solution — Dilute 10 mL of nitric acid with water to 1 L.
9.3.2.4 Indium Internal Standard — Make up an indium internal standard solution in 1% nitric acid to a
concentration of 20 mg/mL from an appropriate indium standard solution.
9.3.3 Sample Preparation for Trace Metals
9.3.3.1 All Elements — In a clean environment, place 200 g of sample into a PTFE dish. Add 100 mL of 1% nitric
acid solution. Slowly evaporate avoiding loss of sample by effervescence or spattering until 1 to 2 mL remain. Add
5 mL 1% nitric acid solution, heat at a low temperature for several minutes to ensure dissolution. Cool to room
2 Dionex, Sunnyvale, CA, (
www.dionex.com) or equivalent
SEMI C41-0705 © SEMI 1978, 2005 6
temperature, dilute to 50 mL with 1% nitric acid, add an appropriate volume of indium internal standard and mix
well. Prepare a reagent blank.
9.3.4 Analysis
9.3.4.1 Using the prepared solutions and reagent blank, analyze all trace metals by ICP-MS using analytical
conditions optimized for each element. Calibration standards are made in 1% nitric acid solution with the same
concentration of indium internal standard as in ¶9.3.3.1.
10 Grade 4 Procedures
NOTE 6: Each laboratory is responsible for verifying the validity of the method within its own operation.
10.1 See §7, which contains procedures for the following tests:
Assay
Color (APHA)
Residue after Evaporation
Water (H
2
O)
10.2 See §9, which contains procedures for the following tests:
Assay of Anions
Assay of Trace Metals
11 Grade 5 Procedures
11.1 This section does not apply to this chemical.
12 VLSI Grade Procedures
12.1 Specific procedures for this grade do not exist. Refer to §7 and §8 for available procedures.
13 Tier A Procedures
13.1 This section does not apply to this chemical.
14 Tier B Procedures
14.1 This section does not apply to this chemical.
15 Tier C Procedures
15.1 This section does not apply to this chemical.
16 Tier D Procedures
16.1 This section does not apply to this chemical.