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ACETONE SEMI C19-0 301 © SEMI 1 978, 2001 3 8.11.3 Anal ysis 8.11.3.1 Us ing the prepared sam ple and re agent blank, analy ze group I elements potass ium (K) an d sodium (Na) by atom ic absorption spectroscopy a nd all …

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SEMI C19-0301 © SEMI 1978, 2001 ACETONE2
phenolphthalein indicator solution. Add 0.01 N sodium
hydroxide until a slight, pink color persists after
shaking for one-half minute. Add 42 mL (33 g) of the
sample, mix well, and titrate with 0.01 N sodium
hydroxide until the pink color is reproduced. Not more
than 1.0 mL of the sodium hydroxide solution should be
required.
8.4 Alkalinity — Add 25 mL (20 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.
8.5 Residue after Evaporation — Evaporate 253 mL
(200 g) of sample to dryness. Dry at 105°C for 30 min-
utes, cool in a desiccator, and weigh (see SEMI C1,
Section 3.3, Determination of Residue After
Evaporation).
8.6 Water — Add 25 mL of pyridine 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.
% Wate
r
H
2
O
()
=
mL KF rea
g
ent
×
KF facto
r
g
H
2
OmL()
×
100
Wei
g
ht of sam
p
le
g
()
8.7 Solubility in Water — Mix 40 mL of sample with
40 mL of water. Allow to stand for 30 minutes. The
solution should be as clear as an equal volume of water.
8.8 Chloride — To 63 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,
dilute to 20 mL with water, and 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.
8.9 Phosphate — To 125 mL (100 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 as the sample.
8.10 Arsenic and Antimony (as As) — Evaporate 250
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, 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 General Method for Arsenic
(and Antimony) under SEMI C1, Section 3.4.5, starting
with the sentence which begins: "Swirl the 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).
8.11 Trace Metal Analysis — 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), boron (B),
calcium (Ca), chromium (Cr), copper (Cu), gold (Au),
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 appropriate studies demonstrate
recovery between 75 - 125% of a known sample spike
for half of the value of each specified item.
8.11.1 Special Reagents
8.11.1.1 Hydrochloric Acid, Ultra Pure — Use hydro-
chloric acid specified for ultra low metal ion content.
8.11.1.2 Mannitol Powder — Use mannitol specified
for reagent grade (A.C.S.) and determined, via the
reagent blank, to be ultra low metal ion content.
8.11.1.3 5% Mannitol Solution — Dissolve and dilute
5 g of mannitol to 100 mL using water meeting the
criteria for Type E1 in ASTM D5127.
8.11.1.4 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 in
ASTM D5127.
8.11.2 Sample Preparation
8.11.2.1 In a clean environment, place 250 g of sol-
vent in a PTFE dish. Add 0.5 mL of freshly prepared
5% mannitol solution. 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.
ACETONE SEMI C19-0301 © SEMI 1978, 20013
8.11.3 Analysis
8.11.3.1 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 plasma emission spectrometry. Apply, if
necessary, a reagent blank correction to the final
determined value of the sample.
NOTE 3: Due to the uncertainty of acid concentration in the
liquid residue the final concentration can be estimated to be
approximately 2% (v/v).
9 Grade 2 Procedures
9.1 This section does not apply to this chemical.
10 Grade 3 Procedures
10.1 This section does not apply to this chemical.
11 Grade 4 Procedures
11.1 This section does not apply to this chemical.
12 Grade 5 Procedures
12.1 This section does not apply to this chemical.
13 VLSI Grade Procedures
13.1 This section does not apply to this chemical.
14 Tier A Procedures
14.1 This section does not apply to this chemical.
15 Tier B Procedures
15.1 This section does not apply to this chemical.
16 Tier C Procedures
16.1 This section does not apply to this chemical.
17 Tier D Procedures
17.1 This section does not apply to this chemical.
Table 1 Impurity Limits and Other Requirements for Acetone
Previous SEMI Reference # C1.2-96
Grade 1
(Specification)
Assay ([CH
3
]
2
CO) 99.5% min
Color (APHA) 10 max
Acidity
0.3 µeq/g max
Alkalinity
0.5 µeq/g max
Residue after Evaporation 5 ppm max
Water (H
2
O) 0.5% max
Solubility in Water To pass test
Chloride (Cl) 0.2 ppm max
Phosphate (PO
4
) 0.1 ppm max
Aluminum (Al) 0.1 ppm max
Arsenic and Antimony (as As) 0.01 ppm max
Boron (B) 0.1 ppm max
Calcium (Ca) 0.1 ppm max
Chromium (Cr) 0.1 ppm max
Copper (Cu) 0.1 ppm max
Gold (Au) 0.1 ppm max
Iron (Fe) 0.1 ppm max
Lead (Pb) 0.1 ppm max
Magnesium (Mg) 0.1 ppm max
Manganese (Mn) 0.1 ppm max
Nickel (Ni) 0.1 ppm max
Potassium (K) 0.1 ppm max
Sodium (Na) 0.1 ppm max
Tin (Sn) 0.1 ppm max
Titanium (Ti) 0.1 ppm max
SEMI C19-0301 © SEMI 1978, 2001 ACETONE4
Previous SEMI Reference # C1.2-96
Grade 1
(Specification)
Zinc (Zn) 0.1 ppm max
Particles in bottles:
size, #/mL
≥1.0 µm, 10 max
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