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SEMI C41-0705 © SEMI 1978, 2005 2 Column: 30 meter × 530 micron I.D. fused silica capillary, coated with 5 micron film of DB-Wax or equivalent (100% methyl silicon e which has been surface bonded and cross linked). Colum…
SEMI C41-0705 © SEMI 1978, 2005 1
SEMI C41-0705
SPECIFICATIONS AND GUIDELINES FOR 2-PROPANOL
This specification was technically approved by the global Liquid Chemicals Committee. This edition was
approved for publication by the global Audits and Reviews Subcommittee on April 7, 2005. It was available
at www.semi.org in June 2005 and on CD-ROM in July 2005. Originally published in 1978; previously
published in 2003.
NOTICE: This document was completely rewritten in 2005.
NOTICE: Paragraphs entitled NOTE are not an official part of this document and are not intended to modify or
supercede it.
1 Purpose
1.1 The purpose of this document is to standardize requirements for 2-propanol used in the semiconductor industry
and testing procedures to support those standards. Test methods have been shown to give statistically valid results.
2 Scope
2.1 The scope of this document covers all grades of 2-propanol used in the semiconductor industry.
2.2 The VLSI grade purity level is typically required by semiconductor devices with geometries of 0.8–1.2 microns.
NOTICE: This standard does not purport to address safety issues, if any, associated with its use. It is the
responsibility of the users of this standard to establish appropriate safety and health practices and determine the
applicability of regulatory or other limitations prior to use.
3 Referenced Standards and Documents
3.1 SEMI Standards
SEMI C1 — Guide for the Analysis of Liquid Chemicals
3.2 ASTM Standards
1
ASTM D5127 — Standard Guide for Ultra Pure Water Used in the Electronics and Semiconductor Industry
NOTICE: Unless otherwise indicated, all documents cited shall be the latest published versions.
4 Terminology
None.
5 Physical Property (for information only)
Density at 25ºC 0.78 g/mL
Boiling Point 82.3ºC
6 Requirements
6.1 The requirements for 2-propanol for Grades 1, 2, 3, 4 & VLSI Guidelines, are listed in Table 1.
7 Grade 1 Procedures
NOTE 1: Each laboratory is responsible for verifying the validity of the method within its own operation.
7.1 Assay — Analyze the sample by gas chromatography (see SEMI C1, ‘Assay by Wide Bore Column Gas
Chromatography’). The parameters cited have given satisfactory results.
1 American Society for Testing and Materials, 100 Barr Harbor Drive, West Conshohocken, Pennsylvania 19428-2959, USA. Telephone:
610.832.9585, Fax: 610.832.9555, www.astm.org
SEMI C41-0705 © SEMI 1978, 2005 2
Column: 30 meter × 530 micron I.D. fused silica capillary, coated with 5 micron film of DB-Wax or equivalent
(100% methyl silicone which has been surface bonded and cross linked).
Column Temperature: 40ºC isothermal for 5 minutes, then programmed to 200ºC at 10ºC/min.
Injector Temperature: 150ºC
Detector Temperature: 250ºC
Sample Size: 0.2 µL splitless
Carrier Gas: Helium at 3 mL/min
Detector: Thermal Conductivity
Approximate Retention Times (min):
Acetone 4.5
2-Propanol 5.0
7.2 Color — Dilute 2.0 mL of platinum-cobalt stock solution (APHA No. 500) to 100 mL with water. Compare this
standard (APHA No. 10) with 100 mL of sample in Nessler tubes. View vertically over a white background. The
sample must be no darker than the standard.
7.3 Acidity — To 25 mL of water in a glass-stoppered flask, add 10 mL of sample and 0.1 mL of phenolphthalein
indicator solution. Add 0.01N sodium hydroxide until a slight pink color persists after shaking for one-half minute.
Add 64 mL (50 g) of the sample, mix well, and titrate with 0.01N sodium hydroxide until the pink color is
reproduced. Not more than 1.0 mL of the sodium hydroxide solution should be required.
7.4 Alkalinity — Add 128 mL (100 g) of sample to 25 mL of water and mix well. Add 0.05 mL of methyl red
indicator solution. Titrate with 0.01 N hydrochloric acid until a slight pink color is produced. Not more than 1.0 mL
of the hydrochloric acid should be required.
7.5 Residue after Evaporation — Evaporate 256 mL (200 g) of sample to dryness. Dry at 105ºC for 30 minutes,
cool in a desiccator, and weigh (see SEMI C1, ‘Residue after Evaporation’).
7.6 Water — Add 25 mL of methanol to a dry titration flask and add Karl Fischer (KF) reagent to a visually or
electrometrically determined endpoint that persists for 30 seconds. Add 25 mL (20 g) of sample, taking care to
protect the sample and contents of the flask from moisture. Stir vigorously and titrate with Karl Fischer reagent to
the same endpoint.
% Water (H
2
O)
mL KF reagent
KF factor g H
2
OmL
100
Weight of sample g
7.7 Solubility in Water — Mix 10 mL of sample with 40 mL of water. Allow to stand 1 hour. The solution should
be as clear as an equal volume of water.
7.8 Chloride — To 64 mL (50 g) of sample, add 10 mL of sodium carbonate reagent solution and evaporate to
dryness on a steam bath in a hood. Dissolve the residue in 10 mL of water, add 1 mL of nitric acid and dilute to 20
mL with water. Add 1 mL of silver nitrate reagent solution. Any turbidity produced should be no greater than that
produced when 0.01 mg of chloride ion (Cl) is treated as the sample.
7.9 Phosphate — To 26 mL (20 g) of sample, add 10 mL of sodium carbonate reagent solution and evaporate to
dryness on a steam bath in a hood. Dissolve the residue in 25 mL of 0.5 N sulfuric acid. Add 1 mL of ammonium
molybdate reagent solution and 1 mL of p-(methylamino)phenol sulfate reagent solution. Allow to stand at room
temperature for 2 hours. Any blue color produced should be no greater than that produced when 0.01 mg of
phosphate ion (PO
4
) is treated like the sample.
7.10 Arsenic and Antimony (as As) — Evaporate 256 mL (200 g) of sample in a 400 mL beaker to a small volume
in a hood. Add 50 mL of water and again evaporate to a small volume. Repeat the evaporation with water addition.
Do not allow to go to dryness. Add 5 mL of nitric acid and 5 mL of sulfuric acid and evaporate to dense fumes of
sulfur trioxide. Cool, cautiously add 10 mL of water, and again evaporate to dense fumes of sulfur trioxide. Cool,
and cautiously wash into a generator flask with water to make a volume of 35 mL. Proceed as described in the
SEMI C1, ‘Trace Arsenic (and Antimony) Determination’, starting with the sentence that begins, “Swirl the
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.