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SEMI C41-0705 © SEMI 1978, 2005 4 8 Grade 2 Procedures NOTE 3: Each labo ratory is responsible fo r verifying the validity of the method within its own operation. 8.1 Non-Metal Impurities — See §7, whi ch cont ains proce…

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SEMI C41-0705 © SEMI 1978, 2005 3
flask....” Any red color in the silver diethyldithiocarbamate solution of the sample should be no greater than that of
the standard containing 0.002 mg of arsenic (As).
7.11 Trace Metal Analysis
7.11.1 Boron — To 128 mL (100 g) of sample, add 0.10 mL of 10% sodium hydroxide, and evaporate to dryness in
a nitrogen atmosphere using a covered chamber such as a Thiers assembly or equivalent. Dissolve the residue with
2 mL of water and 0.10 mL of hydrochloric acid. Transfer to a test tube, cool in an ice bath, and add 10 mL of
sulfuric acid. Add 10 mL of carminic acid solution (¶7.11.1.1) and remove from the ice bath. Allow to stand for 45
minutes. Prepare a standard containing 0.001 mg of boron treated exactly as the sample (¶7.11.1.2). Run a complete
blank determination on 2 mL of water. Measure the absorbances of the sample and standard against the blank at
585 nm using 5.00 cm cells. The absorbance of the sample solution should be no greater than that of the standard.
7.11.1.1 Carminic Acid Solution — Dissolve 0.05 g of carminic acid in 100 mL of sulfuric acid and shake until
dissolution is complete.
7.11.1.2 Boron Standard Solution — Dissolve 0.572 g of boric acid in water in a 1000 mL volumetric flask. Dilute
to the mark with water. Dilute 10.0 mL of this solution with water to the mark in a 100 mL volumetric flask. (1 mL
= 0.01 mg boron.)
7.11.2 Gold (Au) — Analyze by graphite atomic absorption using the manufacturer’s recommended procedure. This
technique has been shown to give satisfactory results using a 1:4 dilution and Zeeman background correction. Each
laboratory must determine the appropriate dilution and background correction for their instrument to meet the
specification limit.
7.11.3 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), chromium (Cr), copper (Cu), 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 they are validated for each trace metal according to
SEMI C1, ‘Method Validation’.
7.11.4 Special Reagents
7.11.4.1 Hydrochloric Acid, Ultra Pure — Use hydrochloric acid specified for ultra low metal ion content.
7.11.4.2 2% (v/v) Hydrochloric Acid Solution — Dilute 20 mL of ultra pure 12 M hydrochloric acid to 1 L using
water meeting the criteria for Type E1.1 in ASTM D5127.
7.11.5 Sample Preparation
7.11.5.1 Tin — To 100 g (128 mL) sample in a PTFE dish add 1 mL of 1% oxalic acid solution. Slowly evaporate
to about 1 mL. Dissolve the residue in 10% hydrochloric acid and transfer to a 10 mL volumetric flask using 10%
hydrochloric acid. Analyze by inductively coupled plasma optical emission spectrometry (ICP-OES) using matrix-
matched standards.
7.11.5.2 All Other Elements — In a clean environment, place 250 g of sample in a PTFE dish. Slowly evaporate on
a hot plate avoiding loss of sample by effervescence or spattering until approximately 1 mL of liquid remains. Take
up liquid and all visible residue (from walls of dish) with 1 mL ultra pure, 12 M hydrochloric acid and continue
heating until approximately 0.5 mL of liquid remains. No undissolved particulate matter should be observed.
Otherwise repeat the addition of hydrochloric acid until all particulate matter is dissolved. Transfer quantitatively to
a 50 mL volumetric flask using 2% (v/v) hydrochloric acid and adjust liquid level to mark. Prepare a reagent blank
using the same reagents and in the same manner as for the sample concentration.
NOTE 2: Due to the uncertainty of acid concentration in the liquid residue, the final concentration can be estimated to be
approximately 2% (v/v). Standard calibration solutions are to use this same acid concentration.
7.11.6 Analysis
7.11.6.1 Using the prepared sample and reagent blank, analyze group I elements potassium (K) and sodium (Na) by
atomic absorption spectroscopy and all other elements by ICP-OES. If necessary, apply a reagent blank correction to
the final determined value of the sample.
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