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METHYL ETHYL KETONE SEMI C32-0699 © SEMI 1 978, 1999 1 SEMI C32-0699 SPECIFICA TION FOR METHYL ETHYL KETONE This spe cifica tion was te chnically approve d by the G lobal Process Che micals Com mittee and is the dire ct …

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SEMI C31-0301 © SEMI 1978, 2001 METHANOL4
Previous SEMI Reference # C1.10-96
Grade 1
(Specification)
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
Zinc (Zn) 0.1 ppm max
Particles in bottles:
size, #/mL
≥ 1.0 µm, 10 max
NOTICE: SEMI makes no warranties or representations as to the suitability of the standards set forth herein for any
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Copyright by SEMI® (Semiconductor Equipment and Materials
International), 3081 Zanker Road, San Jose, CA 95134. Reproduction o
f
the contents in whole or in part is forbidden without express written
consent of SEMI.
METHYL ETHYL KETONE SEMI C32-0699 © SEMI 1978, 19991
SEMI C32-0699
SPECIFICATION FOR METHYL ETHYL KETONE
This specification was technically approved by the Global Process Chemicals Committee and is the direct
responsibility of the North American Process Chemicals Committee. Current edition approved by the North
American Regional Standards Committee on April 23, 1999. Initially available on SEMI OnLine May 1999;
to be published June 1999. This document replaces SEMI C1.11 in its entirety. Originally published in
1978.
1 Purpose
1.1 The purpose of this document is to standardize
requirements for methyl ethyl ketone used in the
semiconductor industry and testing procedures to
support those standards. Test methods have been shown
to give statistically valid results. This document also
provides guidelines for grades of methyl ethyl ketone
for which a need has been identified. In the case of the
guidelines, the test methods may not have been
statistically validated yet.
2 Scope
2.1 The scope of this document is all grades of methyl
ethyl ketone used in the semiconductor industry.
3 Limitations
3.1 None.
4 Referenced Documents
SEMI C1 — Specifications for Reagents
5 Terminology
5.1 None.
6 Physical Property (for information only)
Density at 25°C 0.80 g/mL
Boiling Point 79.6°C
7 Requirements
7.1 The requirements for methyl ethyl ketone for
Grade 1 are listed in Table 1.
8 Grade 1 Procedures
8.1 Assay — Analyze the sample by gas
chromatography (see SEMI C1, Section 3.1, Guidelines
for Assay by Wide Bore Column Gas
Chromatography). The parameters cited have given
satisfactory results.
Column: 30 meter × 530 micron I.D. fused silica
capillary, coated with 5 micron film of DB-1 or
equivalent (100% methyl silicone which has been
surface bonded and cross linked).
Column Temperature: 40°C isothermal for 5 minutes,
then programmed to 200°C at 10°C/min.
Injector Temperature: 150°C
Detector Temperature: 250°C
Sample Size: 0.2 µL splitless
Carrier Gas: Helium at 3 mL/min
Detector:
Thermal
Conductivity
Approximate Retention Times (min):
Methyl Ethyl Ketone 9.0
2-Butanol 10.5
8.2 Color — Dilute 3.0 mL of platinum-cobalt stock
solution (APHA No. 500) to 100 mL with water.
Compare this standard (APHA No. 15) with 100 mL of
sample in Nessler tubes. View vertically over a white
background. The sample must be no darker than the
standard.
8.3 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 0.10 N sodium
hydroxide until a slight, pink color persists after
shaking for one-half minute. Add 21 mL (17 g) of the
sample, mix well, and titrate with 0.01 N sodium
hydroxide until the pink color is reproduced. Not more
than 3.0 mL of the sodium hydroxide solution should be
required.
8.4 Residue After Evaporation — Evaporate 63 mL
(50 g) of sample to dryness. Dry at 105°C for 30
minutes, cool in a desiccator, and weigh (see SEMI C1,
Section 3.3, Determination of Residue After
Evaporation).
8.5 Water — Add 25 mL of pyridi ne-dichloromethane
mixture (1 + 1) 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 rea
g
ent
×
KF factor
g
H
2
OmL
()
×
100
Wei
g
ht of sam
p
le
g
()
SEMI C32-0699 © SEMI 1978, 1999 METHYL ETHYL KETONE2
8.6 Phosphate — To 12.5 mL (10 g) of sample, add 10
mL of sodium carbonate reagent solution and evaporate
to dryness on a steam bath in a hood. Carefully 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 sufate reagent solution. Allow
to stand at room temperature for 2 hours. Any blue
color should be no greater than that produced when
0.01 mg of phosphate ion (PO
4
) is treated as the sample.
8.7 Heavy Metals (as Pb) — Evaporate 25 mL (20 g)
of sample to dryness on a steam bath in a hood.
Dissolve the residue in 3 mL of dilute hydrochIoric acid
(1 + 1) and dilute with water to 15 mL. If necessary,
filter through a small filter, and wash the evaporating
dish and the filter with 10 mL of water. Dilute to 25 mL
with water. For the standard, dilute a solution
containing 0.02 mg of lead ion (Pb) and 3 mL of dilute
hydrochloric acid (1 + 1) to 25 mL with water. Adjust
the pH of both solutions to between 3 and 4 with dilute
ammonium hydroxide (10% NH
3
) or with acetic acid,
and dilute with water to 40 mL. To each solution, add
10 mL of freshly prepared hydrogen sulfide water and
compare. The sample solution should be no darker than
the standard.
8.8 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 and 5 mL of sulfuric acid and
evaporate to dense fumes of sulfur trioxide. Cool and
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).
8.9 Trace Element Contents — By a suitable emission
spectrographic procedure, determine for each of the
specified trace elements that its content is not greater
than the stated specification limit (see SEMI C1,
Section 3.5, Guidelines for Determination of Trace
Elements by Emission Spectrography).
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 Methyl Ethyl Ketone
Previous SEMI Reference # C1.11-95
Grade 1
(Specification)
Assay (CH
3
COCH
2
CH
3
) 99.5% min
Color (APHA) 15 max
Acidity
0.6 µeq/g max
Residue after Evaporation 20 ppm max
Water (H
2
O) 0.2% max