semi合集-English.pdf - 第6642页
n-BUTYL A C ET A T E SEM I C24-0301 © SEMI 1978, 20 01 3 15 Tier B P rocedures 15.1 This section does not apply to t h i s chemical. 16 Tier C P rocedures 16.1 This section does not apply to t h i s chemical. 17 Tier D P…
SEMI C24-0301 © SEMI 1978, 2001 n-BUTYL ACETATE2
15 seconds. Not more than 1.0 mL of the potassium
hydroxide solution should be required.
8.4 Residue after Evaporation — Evaporate 90 mL
(80 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 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 (22 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 (gH
2
O/mL) × 100
Weight of sample (g)
8.6 Phosphate — To 11 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.
8.7 Arsenic and Antimony (as As) — Evaporate 45 mL
(40 g) of sample in a 150 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 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).
8.8 Trace Metal Analysis — The f ollowing 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.
8.8.1 Special Reagents
8.8.1.1 Solution A — Glycerol (ACS Reagent Grade)
10 g, Adipic Acid (99 + %) 1 g, EDTA Acid (ACS
Reagent Grade) 0.1 g. Dilute to 1 L using water
meeting the criteria for Type E1.1 in ASTM D5127.
8.8.1.2 Nitric Acid, Ultra Pure — Use 70% nitric acid
specified for ultra low metal ion content.
8.8.1.3 2% Nitric Acid Solution — Dilute 20 mL of
ultra pure nitric acid to 1 L using water meeting the
criteria for Type E1.1 in ASTM D5127.
8.8.2 Sample Preparation
8.8.2.1 In a clean environment, place 250 g of sample
in a PTFE dish. Add 50 mL of Solution A. Slowly
evaporate in a hot plate avoiding loss of sample by
effervescence or spattering until there is no further loss
of liquid. Cool. Add 1 mL of ultra pure, 70% nitric
acid. While maintaining volume, carefully warm
several minutes to dissolve any residue. Cool. Transfer
quantitatively to a 50 mL volumetric flask using 2%
nitric acid for rinsing and dilution to volume. Run a
reagent blank.
8.8.3 Analysis
8.8.3.1 Using the prepared sample, analyze group I
elements by flame atomic absorption spectroscopy and
all other elements by plasma emission spectroscopy.
Apply, if necessary, a reagent blank correction to the
final determined value of the sample.
NOTE 3: Repeat analysis for tin using larger sample size if
the instrument sensitivity is insufficient at the specified limit.
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.
n-BUTYL ACETATE SEMI C24-0301 © SEMI 1978, 20013
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 n-Butyl Acetate
Previous SEMI Reference # C1.5-96
Grade 1
(Specfication)
Assay (C
6
H
12
O
2
) 99.0% min
Color (APHA) 15 max
Acidity
2.0 µeq/g max
Residue after Evaporation 10 ppm max
Water (H
2
O) 0.05% max
Phosphate (PO
4
) 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
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
particular application. The determination of the suitability of the standard is solely the responsibility of the user.
Users are cautioned to refer to manufacturer’s instructions, product labels, product data sheets, and other relevant
literature respecting any materials mentioned herein. These standards are subject to change without notice.
The user’s attention is called to the possibility that compliance with this standard may require use of copyrighted
material or of an invention covered by patent rights. By publication of this standard, SEMI takes no position
respecting the validity of any patent rights or copyrights asserted in connection with any item mentioned in this
standard. Users of this standard are expressly advised that determination of any such patent rights or copyrights, and
the risk of infringement of such rights, are entirely their own responsibility.
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.
DICHLOROMETHANE (METHYLENE CHLORIDE) SEMI C25-0699
E
© SEMI 1978, 20001
SEMI C25-0699
E
SPECIFICATION FOR DICHLOROMETHANE (METHYLENE CHLORIDE)
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 C1.6 in its entirety. Originally published in 1978.
E
This document was editorially modified in March 2000. Changes were made to the note following Table 1.
1 Purpose
1.1 The purpose of this document is to standardize
requirements for dichloromethane (methylene chloride)
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
dichloromethane 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
dichloromethane 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 1.32 g/mL
Boiling Point 39.8°C
7 Requirements
7.1 The requirements for dichloromethane for Grade 1
are listed in Table 1.
8 Grade 1 Procedures
NOTE 1: Each laboratory is responsible for verifying the
validity of the method within its own operation.
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):
Dichloromethane 6.0
Chloroform 11.0
Carbon Tetrachloride 14.0
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 (50 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 76 mL
(100 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 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 76 mL (100 g) of sample, taking care
to protect the sample and contents of the flask from