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AMMON IUM FLUORIDE 40% SEMI C20-1101 © SEMI 1978, 2001 3 Table 1 Impurity Limits and O ther Requirements for Ammonium Fluoride 40% Previous SEMI Ref erenc e # C1.3-95 C11.2-94 C7.18-9 5 -- Grade 1 VLSI Grade Tier A Tier …

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SEMI C20-1101 © SEMI 1978, 2001 AMMONIUM FLUORIDE 40%2
arsenite reagent solution. Dilute to 50 mL with brucine
sulfate reagent solution and mix. Heat the solution in a
preheated (boiling water) bath for 10 minutes. Cool
rapidly in an ice bath to room temperature. The yellow
color of the sample should be no greater than that
produced when 0.01 mg of nitrate ion (NO
3
) is treated
as the sample.
8.6 Phosphate — To a 9 mL (10 g) sample in a
platinum dish, add 1 mL of sodium carbonate reagent
solution and 40 mL of nitric acid. Evaporate carefully,
to prevent spattering, to near dryness. Cool, wash down
the sides of the dish with 5 mL of nitric acid, and
evaporate to dryness. Repeat the evaporation with nitric
acid two more times to ensure complete removal of all
the fluoride. To the cooled dish, add 25 mL of 0.5 N
sulfuric acid to dissolve the residue, warming if
necessary. Cool, transfer to a color comparison tube,
and add 1 mL of ammonium molybdate reagent solu-
tion, 1 mL of p-(methylamino)phenol sulfate reagent
solution, and allow to stand at room temperature for 2
hours. Any blue color should be no greater than that
produced when 0.01 mg of phosphate ion (PO
4
) is
treated as the sample.
8.7 Sulfate — To 23 mL (25 g) of sample, add 10 mL
of sodium carbonate reagent solution and heat gently
until sample has been volatilized. To the residue add 5
mL of hydrochloric acid 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 for 10 minutes. Any turbidity developed
should be no greater than that produced when 0.05 mg
of sulfate ion (SO
4
) solution is treated as the sample.
8.8 Arsenic and Antimony (as As) — To 30 mL (33 g)
in a fluoroplastic beaker, add 20 mL of nitric acid and 5
mL of hydrochloric acid, and evaporate to dryness in a
sand bath in a hood. Completely volatilize the
ammonium fluoride, but do not bake. Add 10 mL of
water and 5 mL of sulfuric acid and evaporate to dense
fumes 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 that 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 0.001 mg of arsenic (As).
8.9 Trace Element Contents — By a suitable emission
spectrographic procedure, determine for each of the
specified trace elements that its content is not greater
than the stated specification limit (see SEMI C1,
Section 3.5, Guidelines for Emission Spectrography).
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 Specific procedures for this grade do not exist.
Refer to Section 8 for available procedures.
14 Tier A Procedures
14.1 Standardized test methods are being developed for
all parameters at the purity levels indicated. The
Process Chemicals Committee considers a test method
to be valid only if there is a documented recovery study
showing a recovery of 75–125%. Recovery is for a
known sample spike at 50% of the specified level.
15 Tier B Procedures
15.1 Standardized test methods are being developed for
all parameters at the purity levels indicated. The
Process Chemicals Committee considers a test method
to be valid if there is a documented recovery study
showing a recovery of 75–125%. Recovery is for a
known sample spike at 50% of the specified level.
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.
AMMONIUM FLUORIDE 40% SEMI C20-1101 © SEMI 1978, 20013
Table 1 Impurity Limits and Other Requirements for Ammonium Fluoride 40%
Previous SEMI Reference # C1.3-95 C11.2-94 C7.18-95 --
Grade 1 VLSI Grade Tier A Tier B
(Specification) (Guideline) (Guideline) (Guideline)
Assay (NH
4
F) 39.0–41.0% min 39–41% min 39.0–41.0% 39.0–41.0%
Color (APHA) 10 max 10 max 10 max 10 max
Residue after Ignition -- 10 ppm max -- --
pH (1% solution at 25°C)
6.0–7.5 6.2–7.0 6.0–7.5 6.0–7.5
Ammonium Hydrogen Fluoride (NH
4
HF
2
) -- 200 ppm max -- --
Chloride (Cl) 4 ppm max 2 ppm max 2 ppm max 2 ppm max
Nitrate (NO
3
) 10 ppm max 10 ppm max 3 ppm max 3 ppm max
Phosphate (PO
4
) 1 ppm max 0.2 ppm max 0.5 ppm max 0.5 ppm max
Sulfate (SO
4
) 2 ppm max 2 ppm max 2 ppm max 2 ppm max
Aluminum (Al) 0.2 ppm max 0.05 ppm max 10 ppb max 1 ppb max
Antimony (Sb) -- -- 10 ppb max 1 ppb max
Arsenic (As) -- -- 10 ppb max 1 ppb max
Arsenic and Antimony (as As) 0.03 ppm max 0.03 ppm max -- --
Barium (Ba) -- 0.01 ppm max 10 ppb max 1 ppb max
Beryllium (Be) -- 0.01 ppm max -- --
Bismuth (Bi) -- 0.02 ppm max -- --
Boron (B) 0.2 ppm max 0.05 ppm max 10 ppb max 1 ppb max
Cadmium (Cd) -- 0.01 ppm max 10 ppb max 1 ppb max
Calcium (Ca) 0.2 ppm max 0.1 ppm max 10 ppb max 1 ppb max
Chromium (Cr) 0.1 ppm max 0.01 ppm max 10 ppb max 1 ppb max
Cobalt (Co) -- 0.01 ppm max -- --
Copper (Cu) 0.1 ppm max 0.01 ppm max 10 ppb max 1 ppb max
Gallium (Ga) -- 0.01 ppm max -- --
Germanium (Ge) -- 0.05 ppm max -- --
Gold (Au) 0.3 ppm max 0.02 ppm max -- --
Indium (In) -- 0.01 ppm max -- --
Iron (Fe) 0.2 ppm max 0.05 ppm max 10 ppb max 1 ppb max
Lead (Pb) 0.3 ppm max 0.01 ppm max 10 ppb max 1 ppb max
Lithium (Li) -- 0.01 ppm max 10 ppb max 1 ppb max
Magnesium (Mg) 0.2 ppm max 0.05 ppm max 10 ppb max 1 ppb max
Manganese (Mn) 0.2 ppm max 0.01 ppm max 10 ppb max 1 ppb max
Molybdenum (Mo) -- 0.01 ppm max -- --
Nickel (Ni) 0.3 ppm max 0.01 ppm max 10 ppb max 1 ppb max
Platinum (Pt) -- 0.05 ppm max -- --
Potassium (K) 0.3 ppm max 0.05 ppm max 10 ppb max 1 ppb max
Silicon (Si) -- 200 ppm max 3000 ppb max
(See NOTE 1.)
--
Silver (Ag) -- 0.05 ppm max -- --
Sodium (Na) 0.3 ppm max 0.1 ppm max 10 ppb max 1 ppb max
Strontium (Sr) -- 0.01 ppm max -- --
Thallium (Tl) -- 0.02 ppm max -- --
Tin (Sn) 0.2 ppm max 0.02 ppm max 10 ppb max 1 ppb max
Titanium (Ti) 0.3 ppm max 0.01 ppm max 10 ppb max 1 ppb max
Vanadium (V) -- 0.01 ppm max 10 ppb max 1 ppb max
Zinc (Zn) 0.2 ppm max 0.05 ppm max 10 ppb max 1 ppb max
Zirconium (Zr) -- 0.01 ppm max -- --
SEMI C20-1101 © SEMI 1978, 2001 AMMONIUM FLUORIDE 40%4
Previous SEMI Reference # C1.3-95 C11.2-94 C7.18-95 --
Grade 1 VLSI Grade Tier A Tier B
(Specification) (Guideline) (Guideline) (Guideline)
Particles in bottles:
size, #/mL
≥ 1.0 µm, 25 max ≥ 0.5 µm, 250 max
See NOTE 2. See NOTE 2.
NOTE 1: For III-V compound users only.
NOTE 2: Due to the limitations of current particle counters, particle size and number are to be agreed upon between supplier and user. See SEMI
C1, Section 3.9 for particle counting methodology.
NOTICE: SEMI makes no warranties or representations as to the suitability of the standard 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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the risk of infringement of such rights, are entirely their own responsibility.
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