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DICHLOROM ETH A NE (M ETHYLENE CHLORIDE) SEMI C25-0699 E © SEMI 19 78, 2000 3 12 Grade 5 P rocedu res 12.1 This section does not apply to t h i s chemical. 13 VLSI G rade Pro cedures 13.1 This section does not apply to t…
SEMI C25-0699
E
© SEMI 1978, 2000 DICHLOROMETHANE (METHYLENE CHLORIDE)2
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
30 mL (40 g) of sample and 40 mL of water. Shake
well for 30 seconds and allow the two layers to
separate. Discard the sample (lower) 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 0.01 mg of chloride ion (Cl) in an equal
volume of solution containing the amounts of reagents
used.
8.7 Phosphate — To 7.5 mL (10 g) of sample, add 10
mL of sodium carbonate reagent solution and evaporate
to dryness on a steam bath in a hood. 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.
8.8 Heavy Metals (as Pb) — Evaporate 75 mL (100 g)
of sample to dryness on a steam bath in a hood.
Dissolve the residue in 3 mL of diluted hydrochloric
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 diluted hydrochloric acid (1 + 1) to 25 mL with
water. Adjust the pH of both solutions to between 3 and
4 with diluted 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.
8.9 Arsenic and Antimony (as As) — Evaporate 152
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 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).
8.10 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.
8.10.1 Special Reagents
8.10.1.1 Mixed Acid — Mix one volume of ultra pure
70% nitric acid with four volumes of ultra pure 37%
hydrochloric acid.
8.10.1.2 Standards — Composite standards containing
0.5 ppm of each element in 10% v/v mixed acid
solution are stable for at least 60 days.
8.10.2 Sample Preparation — Place 2.5 mL of mixed
acid into a clean 400 mL PTFE beaker. Weigh in 200 g
of sample. Put a PTFE-coated stir bar in the solution
and put the beaker in a hood. Evaporate the sample
under a current of air, meeting class 100 cleanroom
specifications, with stirring to ensure continuous
contact of the acid and sample. Do not heat the sample
to minimize the loss of volatile organo-metallics.
Continue to evaporate until near dryness. Add 2.5 mL
of mixed acid, mix carefully, and transfer the solution
to a 25 mL volumetric flask. Rinse the beaker and
dilute to volume with water.
8.10.3 Analysis
8.10.3.1 Analyze the sample by plasma emission
spectrometry except sodium and potassium by atomic
absorption or flame emission within 24 hours of
dilution using matrix matched standards. Run a reagent
blank and correct the data as necessary.
NOTE 2: The trace metal analysis procedure is provisional,
pending second source verification of recovery data. To be
completed.
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.
DICHLOROMETHANE (METHYLENE CHLORIDE) SEMI C25-0699
E
© SEMI 1978, 20003
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 Dichloromethane (Methylene Chloride)
Previous SEMI Reference # C1.6-96
Grade 1
(Specification)
Assay (CH
2
Cl
2
) 98.0% min
Color (APHA) 10 max
Acidity
0.2 µeq/g
Residue after Evaporation 10 ppm max
Chloride (Cl) 0.5 ppm max
Heavy Metals (as Pb) 0.2 ppm max
Phosphate (PO
4
) 1 ppm max
Water (H
2
O) 0.01% max
Aluminum (Al) 1 ppm max
Arsenic and Antimony (as As) 0.01 ppm max
Barium (Ba) 1 ppm max
Boron (B) 0.2 ppm max
Cadmium (Cd) 1 ppm max
Calcium (Ca) 1 ppm max
Chromium (Cr) 0.5 ppm max
Cobalt (Co) 0.1 ppm max
Copper (Cu) 0.1 ppm max
Gallium (Ga) 0.5 ppm max
Germanium (Ge) 1 ppm max
Gold (Au) 0.5 ppm max
Iron (Fe) 1 ppm max
Previous SEMI Reference # C1.6-96
Grade 1
(Specification)
Lithium (Li) 1 ppm max
Magnesium (Mg) 1 ppm max
Manganese (Mn) 1 ppm max
Nickel (Ni) 0.1 ppm max
Potassium (K) 1 ppm max
Silicon (Si) 1 ppm max
Silver (Ag) 0.5 ppm max
Sodium (Na) 1 ppm max
Strontium (Sr) 1 ppm max
Tin (Sn) 1 ppm max
Zinc (Zn) 1 ppm max
NOTE: Dichloromethane contains 0.0025−0.05% ethanol,
cyclohexane, or mixed pentenes as stabilizer.
NOTICE: These standards do not purport to address
safety issues, if any, associated with their use. It is the
responsibility of the user of these standards to establish
appropriate safety and health practices and determine
the applicability of regulatory limitations prior to use.
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.
HEXAMETHYLDISILAZANE SEMI C26-0699
E
© SEMI 1983, 20001
SEMI C26-0699
E
SPECIFICATION AND GUIDELINE FOR HEXAMETHYLDISILAZANE
(HMDS)
This specification and guideline were technically approved by the Global Process Chemicals Committee and
are 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 C1.23 and C7.10 in their
entirety. Originally published in 1983 and 1991 respectively.
E
This document was editorially modified in April 2000 to correct a formatting error. Changes were made to
Table 1.
1 Purpose
1.1 The purpose of this document is to standardize
requirements for hexamethyldisilazane 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 hexamethyldisilazane
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
hexamethyldisilazane 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 Properties (for in formation only)
Density at 25°C
0.77 g/mL
Boiling Point
126°C
7 Requirements
7.1 The requirements for hexamethyldisilazane for
Grade 1 and Tier A 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 Columns Gas
Chromatography). The parameters cited have given
satisfactory results.
Column: 30 meter × 530 micon I.D. fused silica
capillary, coated with 5 micron film of DB-1 or
equivalent (100% methylsilicone which has been
bonded and cross linked).
Column Temperature: 40°C isothermal for 2 minutes,
then programmed to 220°C at 10°C/min, and isothermal
for 10 minutes.
Injector Temperature:
200°C
Detector Temperature:
300°C
Sample Size:
0.4 µL
Carrier Gas: Helium at 8 mL/min
Detector: Thermal Conductivity
Approximate Retention Times (min):
Hexamethyldisilazane 14.3
8.2 Trailing Impurities — Use the chromatogram
developed in the assay (see Section 8.1). With the
relative retention time for hexamethyldisilazane taken
as 1.0, establish the integrated area percents for trailing
impurities with relative retention times from 1.3 to 4.0.
The total of such trailing impurities should not exceed
0.1%.
8.3 Appearance — Place 15 mL of the sample in a 20
× 150 mm test tube and compare with water in a similar
tube. Viewed across the column by means of
transmitted light, the two liquids should be equal in
clarity and free from suspended matter.
8.4 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 should be no darker than the
standard.
8.5 Residue After Evaporation — Evaporate 130 mL
(100 g) of sample to dryness in a hood. Dry at 105°C
for one hour, cool in a desiccator, and weigh (see SEMI
C1, Section 3.3, Determination of Residue After
Evaporation).