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SEMI C53-0704 © SEMI 2001, 2004 DIMET H YL SUL F O XIDE 2 remaining after evaporati o n of a sampl e of DMSO followed by heating of the residue: Heat a clean 200 mL beaker at 105°C in an ov en for 30 min., cool for 30 mi…

SEMI C53-0704 © SEMI 2001, 2004 1

DIMETHYL SULFOXIDE

SEMI C53-0704

SPECIFICATIONS FOR DIMETHYL SULFOXIDE (DMSO) [GRADES 1

AND 2]

These specifications were technically approved by the Global Liquid Chemicals Committee and are the direct

responsibility of the European Liquid Chemicals Committee. Current edition approved by the European

Regional Standards Committee on April 30, 2004. Initially available at www.semi.org June 2004; to be

published July 2004. Originally published November 2001; previously published November 2002.

1 Purpose

1.1 The purpose of this document is to standardize

requirements for dimethyl sulfoxide used in the

semiconductor industry and testing procedures to

support those standards. Test methods have been shown

to give statistically valid results.

2 Scope

2.1 The scope of this document is all grades of DMSO

used in the semiconductor industry.

NOTICE: This standard does not purport to address

safety issues, if any, associated with its use. It is the

responsibility of the users of this standard to establish

appropriate safety and health practices and determine

the applicability of regulatory or other limitations prior

to use.

3 Limitations

3.1 None.

4 Referenced Standards

4.1 SEMI Standards

SEMI C1 — Guide for the Analysis of Liquid

Chemicals

NOTICE: Unless otherwise indicated, all documents

cited shall be the latest published versions.

5 Terminology

5.1 None.

6 Physical Property (for information only)

Density (d 20/4) 1.10 g/mL

7 Requirements

7.1 The requirements for dimethyl sulfoxide for grades

1 and 2 are listed in Table 1.

8 Grade 1 and Grade 2 Procedures

8.1 Assay — Analyze the sample by gas

chromatography (see SEMI C1, Guidelines for Assay

by Wide Bore Column Gas Chromatography). The

parameters cited have given satisfactory results.

8.1.1 Column — 50 meter × 320 micron I.D. fused

silica capillary, coated with 5 micron film of OV-1 or

equivalent (100% methyl silicone which has been

surface bonded and cross linked).

Column Temperature: 135°C isothermal

Injector Temperature: 240°C

Detector Temperature: 280°C

Sample Size: 1 µl

Carrier Gas: Helium at 1.2 mL/min.

Detector: Flame ionization

Approximate Retention Times

(min):

Dimethylsulfide 3.8

Dimethylsulfoxide 10.9

Dimethylsulfone 14.1

8.2 Color — Using a colorimeter, compare sample in a

specific glass tube with flat bottom, graduated at 113

and 250 mm, with a standardized color reference disk

CAA (Scale 2.5 to 30 APHA units).

8.3 Water  Use a Karl Fischer (KF) coulometer,

consisting of a titration beaker, an electrode generator

and an electrode indicator with double platinum wire;

having as reagents Hydranal Coulomat A solution at the

anode and Hydranal Coulomat C solution at the

cathode. Add 500 µl of sample, taking care to protect

the sample from moisture. Read directly the water

content of sample in µg of water.

8.4 Acidity  Use a potentiograph with a compound

glass electrode and a titration vat with nitrogen inlet. To

100 mL of sample add 5 mL of water, 5 mL of

methanol and 2 drops of titan yellow under nitrogen-

stream. The titration is performed with N/100

tetrabutylammonium hydroxide (TBAH) in

isopropanol. The equivalence point is at about −400

mV. The density (see SEMI C1) of the Dimethyl

sulfoxide sample to be titrated must be determined to

express the result in (meq/g).

8.5 Residue after Evaporation



The residue after

evaporation is defined as the relative amount of residue

SEMI C53-0704 © SEMI 2001, 2004 DIMETHYL SULFOXIDE 2

remaining after evaporation of a sample of DMSO

followed by heating of the residue: Heat a clean 200

mL beaker at 105°C in an oven for 30 min., cool for 30

min. in a dessicator charged with calcium chloride and

weigh. Place 100 g of DMSO into the 200 mL tared

beaker. Evaporate the liquid gently, so that boiling does

not occur, in a hood protected from any possibility of

contamination. When all the sample has evaporated, dry

the residue in an oven at 105°C for 30 minutes and cool

the beaker for 30 min in a dessicator charged with

calcium chloride and reweigh.

8.5.1 Calculate the residue as parts per million (ppm).

8.6 Trace Metal Determination — 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), antimony

(Sb), arsenic (As), barium (Ba), boron (B), cadmium

(Cd), calcium (Ca), chromium (Cr), copper (Cu), iron

(Fe), lead (Pb), lithium (Li), magnesium (Mg),

manganese (Mn), nickel (Ni), potassium (K), sodium

(Na), tin (Sn), titanium (Ti), vanadium (V) and zinc

(Zn). Alternate methods may be used as long as the

method has been validated according to SEMI C1.

8.7 Special Reagents

8.7.1 Water — The water used for all the dilution,

calibration, and standards should meet suggested

guidelines for pure water for semiconductor processing.

8.7.2 Sample Preparation — In a clean environment,

dilute 25 mL of sample by adding 25 mL of water.

Prepare reagent blanks.

8.7.3 Analysis — Using the prepared sample and

reagent blanks, analyze the elements by inductively

coupled plasma (ICP). The density (see SEMI C1) of

the DMSO sample must be determined to express the

result in ppb.

8.7.4 Notes

NOTE 1: Each laboratory is responsible for verifying the

validity of the method within its own operation.

Table 1 Impurity Limit and Other Requirements for

Dimethyl Sulfoxide

Grade 1 Grade 2

(specification) (specification)

Assay (CH

SOCH

) 99.8% min. 99.8% min.

DMSO

(CH

)

0.05% max. 0.05% max.

DMS (CH

SCH

) 0.05% max. 0.05% max.

Color (APHA) 10 max. 10 max.

Water (H

O) 0.05% max. 0.05% max.

Acidity 0.0007 meq/g max. 0.0007 meq/g

max.

Grade 1 Grade 2

(specification) (specification)

Residue after

evaporation (ppm)

50 50

Aluminum (Al) 50 ppb max. 10 ppb max.

Antimony (Sb) 50 ppb max. 10 ppb max.

Arsenic (As) 50 ppb max. 10 ppb max.

Barium (Ba) 50 ppb max. 10 ppb max.

Boron (B) 50 ppb max. 10 ppb max.

Cadmium (Cd) 50 ppb max. 10 ppb max.

Calcium (Ca) 50 ppb max. 10 ppb max.

Chromium (Cr) 50 ppb max. 10 ppb max.

Copper (Cu) 50 ppb max. 10 ppb max.

Iron (Fe) 50 ppb max. 10 ppb max.

Lead (Pb) 50 ppb max. 10 ppb max.

Lithium (Li) 50 ppb max. 10 ppb max.

Magnesium (Mg) 50 ppb max. 10 ppb max.

Manganese (Mn) 50 ppb max. 10 ppb max.

Nickel (Ni) 50 ppb max. 10 ppb max.

Potassium (K) 50 ppb max. 10 ppb max.

Sodium (Na) 50 ppb max. 10 ppb max.

Tin (Sn) 50 ppb max. 10 ppb max.

Titanium (Ti) 50 ppb max. 10 ppb max.

Vanadium (V) 50 ppb max. 10 ppb max.

Zinc (Zn) 50 ppb max. 10 ppb 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 or equipment mentioned

herein. These standards are subject to change without

notice.

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