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SEMI C43-0699 © SEM I 1999 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 rocedures 17.1 This section…

SEMI C43-0699 © SEMI 1999 SODIUM HYDROXIDE, 50% SOLUTION2

hydrochloric acid. For the standard, take 50 mL of

water in a similar flask, and add 10 mL of the stock

solution and 1 mL of the nitrogen standard solution

(0.010mg N/ml). To each flask add 0.5 g of aluminum

wire in small pieces, and allow the solution to stand for

1 hour. Slowly distill to about 35 mL of solution. To

each distillate add 2 mL of freshly boiled 10% sodium

hydroxide reagent solution, dilute with water to 50 mL

and add 2 mL of Nessler reagent. Any color in the

solution of the sample should not exceed that in the

standard.

8.7 Chloride  Dilute l0 mL of th e stock solution

with water to 100 mL. Filter, if necessary, through a

chloride-free filter. To 25 mL of this solution, add 5

mL of water, 1 mL of nitric acid, and 1 mL of silver

nitrate reagent solution. Any turbidity developed

should not exceed that produced by 0.01 mg of chloride

(CI) ion in an equal volume of solution containing the

quantities of reagent used in the test

8.8 Phosphate  To 40 mL of the stock solution, add

10 mL of hydrochloric acid and evaporate to dryness on

a steam bath. Dissolve the residue in 25 mL of 0.5 N

sulfuric acid. Add 1 mL of ammonium molybdate

reagent solution and l mL of p-(methylamino)phenol

sulfate reagent solution. Allow the solution to stand for

2 hours at room temperature. Any blue color developed

should not exceed that produced when 0.02 mg of

phosphate (PO

) ion is treated as the sample.

8.9 Sulfate  To 40 mL of the stock solution, add 5

mL of hydrochloric acid and evaporate to dryness on a

steam bath. Dissolve the residue in 20 mL of water and

evaporate again to dryness. Dissolve the residue in 20

mL of water, filter if necessary, and add 1 mL of dilute

hydrochloric acid (1+19) and 1 mL of barium chloride

reagent solution. Allow the solution to stand for 10

minutes. Any turbidity developed should not exceed

that produced when 0.04 mg of sulfate (SO

) ion is

treated as the sample.

8.10 Heavy Metals (as Ag)  To 60 mL of the stock

solution cautiously add 20 mL of nitric acid. For the

standard add 0.05 mg of silver ion (Ag) to 10 mL of the

stock solution and cautiously add 20 mL of nitric acid.

Evaporate both solutions to dryness over a low flame or

on an electric hot plate. Dissolve each residue in about

20 mL of water, filter if necessary through a chloride-

free filter, and dilute with water to 25 mL. Adjust the

pH of the standard and sample solutions to between 3

and 4 (using a pH meter) with 1 N acetic acid or

ammonium hydroxide (10% NH

). Dilute each solution

with water to 40 mL and stir. Add 10 mL of freshly

prepared hydrogen sulfide water to each solution and

stir again. Any color developed in the sample should

not exceed that in the standard.

8.11 Iron  Neutralize 20 mL of the stock solution

with hydrochloric acid, using a phenolphthalein

indicator solution, add 2 mL of HCI in excess, and

dilute with water to 50 mL. Add 30 to 50 mg of

ammonium peroxydisulfate crystals and 3 mL of

ammonium thiocyanate reagent solution. Any red color

developed should not exceed that produced when 0.01

mg of iron (Fe) ion is treated as the sample.

8.12 Nickel  Dilute 40 mL of the stock solution to

50 mL with water and neutralize with hydrochloric acid

using a pH meter. Dilute to 85 mL with water and add

ammonium hydroxide to make the solution barely basic

(pH 8). Add 5 mL of bromine water and 5 mL of

alcoholic 1% dimethylgy1oxime solution in alcohol,

and 5 mL of 10% sodium hydroxide reagent solution.

Any red color developed should not exceed that

produced when 0.02 mg of nickel (Ni) ion is treated as

the sample.

8.13 Potassium  Dilute 10 mL of the stock solution

with water to 100 mL to form the sample solution. To

prepare the standard solution, add 0.1 mg of potassium

(K) ion to 10 mL of the stock solution and dilute with

water to 100 mL.

8.13.1 Using flame emission spectroscopy, observe

the emission of the standard solution at the 767 nm

potassium line. Observe the emission of the sample

solution at the 767 nm potassium line and also at a

wavelength of 750 nm. The difference between the

intensities observed for the Sample Solution at 767 nm

and 750 nm should not exceed the difference observed

at 767 nm between the sample solution and standard

solution (see SEMI Cl, Section 3.7, Flame Emission

Spectroscopy).

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.

SEMI C43-0699 © SEMI 19993

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 Sodium Hydroxide, 50% Solution

Previous SEMI Reference # --

Grade 1

(Specification)

Assay (NaOH) 50.0 - 52.0%

Ammonium Hydroxide

Precipitate

0.01% max

Insoluble Matter 50 ppm max

Nitrogen Compounds (as N) 5 ppm max

Chloride (Cl) 40 ppm max

Phosphate (PO

) 5 ppm max

Sodium Carbonate (Na

)0.1% max

Sulfate (SO

) 10 ppm max

Heavy Metals (as Ag) 10 ppm max

Iron (Fe) 5 ppm max

Nickel (Ni) 5 ppm max

Potassium (K) 0.01% 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.

SULFURIC ACID SEMI C44-0301 © SEMI 1978, 20011

SEMI C44-0301

SPECIFICATIONS AND GUIDELINES FOR SULFURIC 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 on October 17, 1999. Initially available at

www.semi.org February 2001; to be published March 2001. This document replaces SEMI C1.16, C7.8,

C8.8, and C11.5 in their entirety. Originally published in 1978, 1990, 1992, and 1994 respectively;

previously published October 2000.

1 Purpose

1.1 The purpose of this document is to standardize

requirements for sulfuric 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 sulfuric 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 sulfuric

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 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 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

1.83 g/mL

7 Requirements

7.1 The requirements for sulfuric 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 1 mL of sample in a

small glass-stoppered conical flask. Cautiously add 30

mL of water, cool, add 0.1 mL of methyl orange

indicator solution, and titrate with standardized 1.0 N

sodium hydroxide to a red to yellow color change.

%Assay

of NaOH

4.904

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 Chloride — Place 40 mL of water in each of two

beakers. To one, add carefully 27 mL (50 g) of sample

and to the other, 27 mL (50 g) of chloride-free sulfuric

acid and 0.005 mg of chloride ion (Cl). Cool to room

temperature and add 1 mL of nitric acid and 1 mL of

silver nitrate reagent solution. Mix well; if necessary,

make the volume of each solution identical by adding

water. After 10 minutes, measure the turbidity of each

solution using a suitable nephelometer. The turbidity in

the sample should be no greater than the standard.

NOTE 3: Prepare chloride-free sulfuric acid in a hood by

gently fuming sulfuric acid in a crucible or dish for at least 30