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SEMI C42-0699 © SEMI 1978, 1999 SODIUM HYDRO XIDE PELLETS 2 mL. To each d istillate, add 2 mL of freshly boiled 10% sodium hydroxide reagent solutio n, dilute with water to 50 mL , and add 2 mL of Nessler reagent. Any co…

SODIUM HYDROXIDE PELLETS SEMI C42-0699 © SEMI 1978, 19991

SEMI C42-0699

SPECIFICATION FOR SODIUM HYDROXIDE PELLETS

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 C1.22 in its entirety. Originally published in

1978.

1 Purpose

1.1 The purpose of this document is to standardize

requirements for sodium hydroxide pellets 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 sodium hydroxide

pellets 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 sodium

hydroxide pellets 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)

6.1 Not applicable.

7 Requirements

7.1 The requirements for sodium hydroxide pellets for

Grade 1 are listed in Table 1.

8 Grade 1 Procedures

8.1 Assay — Weigh accurately 35 to 40 g of sample in

a closed weighing bottle. Transfer to a 500 mL

volumetric flask, dissolve with carbon dioxide-free

water, cool to 25°C, dilute to the mark with carbon

dioxide-free water, and mix thoroughly. Transfer 25

mL of this solution to a 500 mL glass-stoppered flask,

dilute with 175 mL of carbon dioxide-free water, add 5

mL of barium chloride reagent solution, shake, and

allow to stand for five minutes. Add 0.15 mL of

phenolphthalein indicator solution and titrate with 1 N

hydrochloric acid. (Save this solution for the sodium

carbonate test.)

%Assay

of HCl

80.0

Weight of sample g

(

)

8.2 Sodium Carbonate (Na

) — To the above

titrated solution, add 0.15 mL of methyl orange

indicator and continue the titration with 1 N

hydrochloric acid, making sure that no insoluble

carbonate remains. The additional hydrochloric acid is

equivalent to that consumed by the sodium carbonate.

% Na

of HCl

106.00

Weight of sample g

(

)

8.3 Ammonium Hydroxide Precipitate — Weigh 10 g

of sample and dissolve in about 100 mL of water.

Cautiously add 15 mL of sulfuric acid to 15 mL of

water, cool; then cautiously add the mixture to the

solution of the sample, and evaporate to dense fumes.

Cool, dissolve the residue in 130 mL of hot water, and

add ammonium hydroxide until the solution is just basic

to methyl red. Heat to boiling, filter, wash with hot

water, and ignite. The weight of the residue should not

exceed 2 mg.

8.4 Insoluble Matter — Dissolve 50 g of sample in

250 mL of carbon dioxide-free water in a 500 mL

stoppered flask and cool to 25° C. The solution should

be clear and colorless. Filter through a tared, medium-

porosity filtering crucible and wash thoroughly with hot

water. Dry at 105° C for 1 hour, cool, and weigh the

residue. The result of the residue should not exceed 2.5

mg.

8.5 Stock Solution for 8.6-8.11, 8.13-8.14 — Dissolve

50 g of sample in 250 mL of carbon dioxide-free water

and dilute with such water to 500 mL. One mL contains

0.10 g of sample. Store in a plastic container.

8.6 Nitrogen Compounds (as N) — Dilute 20 mL of

the Stock Solution with 50 mL of water in a flask

connected through a spray trap to a condenser, the end

of which dips beneath the surface of 10 mL of 0.1 N

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. To

each flask add 0.5 g of aluminum wire in small pieces,

allow to stand for 1 hour, and slowly distill about 35

SEMI C42-0699 © SEMI 1978, 1999 SODIUM HYDROXIDE PELLETS2

mL. 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 10 mL of the Stock Solution

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

chloride-free filter. To 20 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 ion (Cl) in

an equal volume of solution containing the quantities of

reagents used in the test.

8.8 Phosphate — To 40 mL of 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 1 mL of p-(methylamino)phenol

sulfate reagent solution. Allow to stand for 2 hours at

room temperature. Any blue color developed should not

exceed that produced when 0.02 mg of phosphate ion

(PO

) is treated as the sample.

8.9 Sulfate — To 20 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 to stand for 10 minutes. Any

turbidity developed should not exceed that produced

when 0.04 mg of sulfate ion (SO

) 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 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 10 mL of the Stock Solution

with hydrochloric acid using phenolphthalein indicator

solution, add 2 mL in excess, and dilute with water to

50 mL. Add 30 to 50 mg of ammonium peroxydisulfate

crystals and 3 mL of ammonium theiocyanate reagent

solution. Any red color developed should not exceed

that produced when 0.01 mg of iron ion (Fe) is treated

as the sample.

8.12 Mercury — To each of two thoroughly clean 125

mL conical flasks add 20 mL of water and 1 mL of 4%

potassium permanganate solution. To one add 5.5 g of

sample. To the other add 0.5 g of sample and 0.5 mg of

mercury ion (Hg). To each flask slowly add 18 mL of

hydrochloric acid, with constant swirling. Heat to

boiling, allow to cool, and dilute to 100 mL. Determine

mercury in 10 mL aliquots by the cold vapor

(flameless) atomic absorption method using 1 mL of

10% hydroxylamine hydrochloride reagent solution and

2 mL of 10% stannous chloride reagent solution for the

reduction. The peak obtained with the sample solution

should not be larger than that of the standard mercury

solution.

8.13 Nickel — Dilute 20 mL of the Stock Solution to

50 mL with water and neutralize with hydrochloric acid

using a pH meter. Dilute to 85 mL and add ammonium

hydroxide to make the solution just basic (pH 8). Add 5

mL of bromine water, 5 mL of alcoholic 1%

dimethylgyloxime 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 ion (Ni) is treated as the sample.

8.14 Potassium — Dilute 10 mL of the Stock Solution

with water to 100 mL to form the Sample Solution. To

prepare the Standard Solution, add 0.2 mg of potassium

ion (K) to 10 mL of the Stock Solution and dilute with

water to 100 mL.

8.14.1 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 C1, 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.

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 Pellets

Previous SEMI Reference # C1.22-95

Grade 1

(Specification)

Assay (NaOH) 97.0% min

Sodium Carbonate (Na

)0.5% max

Ammonium Hydroxide Precipitate 0.02% max

Insoluble Matter 50 ppm max

Nitrogen Compounds (as N) 10 ppm max

Chloride (Cl) 50 ppm max

Phosphate (PO

) 5 ppm max

Sulfate (SO

) 20 ppm max

Heavy Metals (as Ag) 10 ppm max

Iron (Fe) 10 ppm max

Mercury (Hg) 0.1 ppm max

Nickel (Ni) 10 ppm max

Potassium (K) 0.02% 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.

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