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XYLENES SEMI C51-0699 © SEMI 1 978, 1999 1 SEMI C51-0699 SPECIFICA TION FOR XYLENES This spe cifica tion was te chnically approve d by the G lobal Process Che micals Com mittee and is the dire ct responsi bility of the N…
SEMI C50-0699 © SEMI 1995, 1999 2
Table 1 Impurity Limits and Other Requirements for Trimethylphosphite
Previous SEMI Reference # C7.22-95
Tier A
(Guideline)
Assay (P(CH
3
O)
3
) 99.0% min
Color (APHA) 10 max
Aluminum (Al) 5 ppb max
Arsenic (As) 10 ppb max
Barium (Ba) 5 ppb max
Bismuth (Bi) 5 ppb max
Calcium (Ca) 5 ppb max
Chromium (Cr) 5 ppb max
Cobalt (Co) 5 ppb max
Copper (Cu) 5 ppb max
Gallium (Ga) 5 ppb max
Gold (Au) 5 ppb max
Iron (Fe) 5 ppb max
Lead (Pb) 5 ppb max
Lithium (Li) 5 ppb max
Magnesium (Mg) 5 ppb max
Manganese (Mn) 5 ppb max
Mercury (Hg) 5 ppb max
Nickel (Ni) 5 ppb max
Potassium (K) 5 ppb max
Silver (Ag) 5 ppb max
Sodium (Na) 15 ppb max
Strontium (Sr) 5 ppb max
Tin (Sn) 5 ppb max
Titanium (Ti) 5 ppb max
Zinc (Zn) 10 ppb max
NOTICE: These standards do not purport to address
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responsibility of the user of these standards to establish
appropriate safety and health practices and determine
the applicability of regulatory limitations prior to use.
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suitability of the standards set forth herein for any
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suitability of the standard is solely the responsibility of
the user. Users are cautioned to refer to manufacturer’s
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other relevant literature respecting any materials
mentioned herein. These standards are subject to
change without notice.
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compliance with this standard may require use of
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takes no position respecting the validity of any patent
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f
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XYLENES SEMI C51-0699 © SEMI 1978, 19991
SEMI C51-0699
SPECIFICATION FOR XYLENES
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 C1.21 in its entirety. Originally published in
1978.
1 Purpose
1.1 The purpose of this document is to standardize
requirements for xylenes 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 xylenes 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 xylenes
used in the semiconductor industry.
2.2 This material is a mixture of ortho, meta, and para
isomers and ethylbenzene. Xylene (o-, m-, and p- iso-
mers and ethylbenzene) 99.0% min and Ethylbenzene
18% max.
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 0.86 g/mL
Boiling Range 136 - 144°C
7 Requirements
7.1 The requirements for xylenes for Grade 1 are listed
in Table 1.
8 Grade 1 Procedures
8.1 Assay — Assay the sample by gas chromatography
(see SEMI C1, Section 3.1, Guidelines for Assay by
Wide Bore 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: 175°C
Detector Temperature: 250°C
Sample Size: 0.2 µL splitless
Carrier Gas: Helium at 3 mL/min
Detector: Thermal Conductivity or
Flame Ionization
Approximate Retention
Times (min):
Toulene 14.4
Ethylbenzene 17.0
p-xylene 16.9
m-xylene 17.2
o-xylene 17.8
8.1.1 Measure the areas under all peaks by any
convenient means and calulate the concentration of all
components in area percent (see SEMI C.1, Section
3.11, Guidelines for Assay by Wide Bore Column Gas
Chromatography).
8.2 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.
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 0.01 N sodium
hydroxide until a slight pink color persists after shaking
for one-half minute. Add 38 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 Residue After Evaporation — Evaporate 232 mL
(200 g) of sample to dryness. Dry at 105°C for 30
minutes, cool in a desiccator, and weigh (see SEMI C1,
SEMI C51-0699 © SEMI 1978, 1999 XYLENES2
Section 3.3, Determination of Residue After
Evaporation).
8.5 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 23 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
O/mL) × 100
Weight of sample (g)
8.6 Chloride — To a 100 mL separatory funnel, add
12 mL (10 g) of sample and 40 mL of water. Shake
well for 30 seconds and allow the two layers to
separate. Discard the sample (upper) layer. To a 20 mL
portion of the water layer add 1 mL of nitric acid and 1
mL of silver nitrate reagent solution. Any turbidity
produced should be no greater than that of a standard
containing 0.015 mg of chloride ion (Cl) in an equal
volume of solution and the amounts of reagents used.
8.7 Phosphate — To 12 mL (10 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
should be no greater than that produced when 0.01 mg
of phosphate ion (PO
4
) is treated as the sample.
8.8 Arsenic and Antimony (as As) — Evaporate 116
mL (100 g) of sample in a 250 mL beaker to a small
volume in a hood. Add 50 mL of water and again
evaporate to a small volume. Repeat the evaporation
three times with water additions. 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
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 0.001 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.