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HYDROCHLORIC ACID SEM I C27-0301 © SEMI 1978, 2001 1 SEMI C27-0301 SPECIFICA TIONS AND GUIDELINES FOR HYDROCHLORIC A CID These specific ations and gui delines were technica lly approv ed by the Global Proc ess Chem ic al…

SEMI C26-0699

Previous SEMI Reference # C1.23-94 C7.10-94

Grade 1 Tier A

(Specification) (Guideline)

Silver (Ag) 0.1 ppm max 10 ppb max

Sodium (Na) 0.5 ppm max 10 ppb max

Strontium (Sr) 0.1 ppm max 10 ppb max

Tantalum (Ta) 0.1 ppm max 10 ppb max

Thallium (Tl) -- 10 ppb max

Tin (Sn) -- 10 ppb max

Titantium (Ti) -- 10 ppb max

Vanadium (V) -- 10 ppb max

Zinc (Zn) -- 10 ppb max

Zirconium (Zr) -- 10 ppb max

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.

International), 3081 Zanker Road, San Jose, CA 95134. Reproduction o

the contents in whole or in part is forbidden without express written

consent of SEMI.

HYDROCHLORIC ACID SEMI C27-0301 © SEMI 1978, 20011

SEMI C27-0301

SPECIFICATIONS AND GUIDELINES FOR HYDROCHLORIC ACID

These specifications and guidelines 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 by letter ballot dated October 17, 1999.

Initially available at www.semi.org February 2001; to be published March 2001. This document replaces

SEMI C1.7, C7.2, C8.2, C11.6, and C12.2 in their entirety. Originally published in 1978, 1990, 1992, 1996,

and 1995 respectively; previously published June 2000.

1 Purpose

1.1 The purpose of this document is to standardize

requirements for hydrochloric acid 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 hydrochloric acid 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

hydrochloric acid used in the semiconductor industry.

2.2 The VLSI grade purity level is typically required

by semiconductor devices with geometries of 0.8–1.2

microns.

2.3 These specifications and guidelines do not purport

to address safety issues, if any, associated with their

use. It is the responsibility of the users of these

specifications and guidelines to establish appropriate

safety and health practices and determine the

applicability of regulatory limitations prior to use.

3 Limitations

3.1 None.

4 Referenced Standards

4.1 SEMI Standards

SEMI C1 — Specifications for Reagents

4.2 ASTM Standards

ASTM D5127 — Standard Guide for Ultra Pure Water

Used in the Electronics and Semiconductor Industry

NOTE 1: As listed or revised, all documents cited shall be the

latest publications of adopted standards.

1 American Society for Testing and Materials, 100 Barr Harbor

Drive, West Conshohocken, Pennsylvania 19428-2959, USA.

Telephone: 610.832.9585, Fax: 610.832.9555. Website:

www.astm.org

5 Terminology

5.1 None.

6 Physical Property (for information only)

Density at 25°C

1.19 g/mL

7 Requirements

7.1 The requirements for hydrochloric acid for Grades

1 and 2, VLSI Grade, and Tiers B and C are listed in

Table 1.

8 Grade 1 Procedures

NOTE 2: Each laboratory is responsible for verifying the

validity of the method within its own operation.

8.1 Assay — Accurately weigh a glass-stoppered

conical flask containing about 30 mL of water. Deliver

from a pipet about 3 mL of sample near the water

surface, stopper immediately, and reweigh. Dilute to

about 50 mL with water, add methyl orange indicator

solution, and titrate with standardized 1 N sodium

hydroxide to a red-to-yellow color change.

%Assa

of NaOH

3.646

Weight of sample g

()

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 Extractable Organic Substances — Cool 110 mL

of sample in an ice bath. Add 5 mL of 2,2,4-

trimethylpentane and 100 mL of water to each of two

250 mL separatory funnels. To a third funnel add 100

mL of water and 5 mL of the standard (see below). To

the first funnel add 100 mL of the cooled sample, and

100 mL of water to each of the remaining two. Stopper,

shake well, and allow the layers to separate. Inject 1.0

µL of each of the 2,2,4-trimethylpentane extracts into a

gas chromatograph with a flame ionization detector.

The following conditions have been found to be

satisfactory: Column — 20% Carbowax 20 M on

SEMI C27-0301 © SEMI 1978, 2001 HYDROCHLORIC ACID2

Chromosorb P (80/100), 3 m × 3 mm stainless steel or

glass; injection port at 280°C with glass insert; column

temperature initially 65°C, programmed at 6°C/min up

to 140°C; carrier gas — nitrogen at 40 mL/min; signal

adjusted to give an 80% full-scale deflection; and

preferably, electronic integration of peak areas. For

DDT: Column — 5% silicone gum SESE-30 on

Chromosorb W (60/80), 1.5 × 3 mm, injection port —

as above; column temperature — isothermal at 205°C;

carrier gas — nitrogen at 75 mL/min, and preferably,

electronic integration of peak areas. The order of

elution is 2,2,4-trimethylpentane, carbon tetrachloride,

benzene, chloroform, 2,2,4-trimethylpentane impurity,

1,2-dichloroethane, chlorobenzene, and dichloro-

benzene. The total area under the impurity peaks from

the sample should be no greater than that from the

blank (extract from second funnel) by more than one-

half the total area under the peaks from the standard

(third funnel), also corrected for the blank.

8.3.1 Standard — Use a syringe to add the volumes of

liquid listed in Table 2 into 300 mL of 2,2,4-

trimethylpentane. Add 25 mg of DDT to the solution.

Dilute to 500 mL with 2,2,4-trimethylpentane. The

2,2,4-trimethylpentane used for both the standard and

the analysis should be free from impurities that interfere

with the chromatographic analysis.

8.4 Free Halogen (as Cl

) — Mix 100 mL of sample

and 100 mL of freshly boiled water and cool. Add 0.1

mL of 2% potassium iodide reagent solution and 1 mL

of carbon disulfide, and mix. The carbon disulfide

should not acquire a pink color in one-half minute.

8.5 Phosphate — To 170 mL (200 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 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

) is treated like the

sample.

8.6 Sulfate — To 84 mL (100 g) of sample, add 10 mL

of sodium carbonate reagent solution and evaporate to

dryness in a hood. Dissolve the residue in 10 mL of

water and 1 mL of dilute hydrochloric acid (1 + 19);

filter, if necessary. Add 1 mL of barium chloride

reagent solution, mix, and allow to stand 10 minutes.

Any turbidity should be no greater than that produced

when 0.05 mg of sulfate ion (SO

) is treated as the

sample.

8.7 Sulfite — Add 1 mL of 10 percent potassium

iodide reagent solution, 5 mL of hydrochloric acid, and

2 mL of starch indicator solution to 400 mL of oxygen-

free water. Add 0.01 N iodine until a faint permanent

blue color is produced. Add 85 mL of the sample and

titrate with 0.01 N iodine to the same endpoint. Not

more than 0.20 mL should be required.

8.8 Arsenic and Antimony (as As) — To 168 mL (200

g) of sample in a 400 mL beaker, add 10 mL of nitric

acid and 5 mL of sulfuric acid, and evaporate to dense

fumes of sulfur trioxide in a hood. 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 tile sentence which begins: “Swirl the flask....”

Any red color in the silver diethyldithiocarbamate

solution from the sample should be no greater than that

of the standard containing 0.001 mg of arsenic (As).

8.9 Trace Metal Analysis — The following method

has given satisfactory results in determing 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.

8.9.1 Special Reagents

8.9.1.1 Nitric Acid, Ultra Pure — Use nitric acid

specified for ultra low metal ion content.

8.9.1.2 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.

8.9.2 Sample Preparation

8.9.2.1 In a clean environment, place 250 mL of

sample in a PTFE evaporating dish. Slowly evaporate

on a hot plate, avoiding loss of sample by effervescence

or spattering until approximately 2 mL of liquid

remains. Note: Evaporation typically requires 2 1/2 to 4

hours. Cool. Transfer quantitatively to a 50 mL

volumetric flask using 2% nitric acid for rinsing and

dilution to volume. Run a reagent blank.

8.9.3 Analysis

8.9.3.1 Using the acid sample and reagent blank,

analyze group 1 elements by flame atomic absorption

spectroscopy and all other elements by plasma emission

spectroscopy.