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NITRIC ACID SEMI C35-0301 © SEMI 1979, 20 01 3 9.2.3 Sam ple Preparat ion 9.2.3.1 In a clean env ironment, place 2 . 00 g o f sam p le into a tared FEP bottle (30 mL), dilute with Type E1.1 wat er to a fin al weight of 2…

100%1 / 7923
SEMI C35-0301 © SEMI 1979, 2001 NITRIC ACID2
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
) is treated
as the sample.
8.6 Arsenic and Antimony (as As) — To 141 mL (200
g) of sample in a 400 mL beaker add 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 the sentence
which 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).
8.7 Trace Metal Analysis
8.7.1 Gold (Au) — Analyze by graphite atomic
absorption using the manufacturer's recommended
procedure. This technique has been shown to give
satisfactory results using a 1:4 dilution and Zeeman
background correction. Each laboratory must determine
the appropriate dilution and background correction for
its instrument to meet the specification limit.
8.7.2 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), boron (B), calcium (Ca), chromium
(Cr), copper (Cu), 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.
8.7.3 Special Reagents
8.7.3.1 Nitric Acid, Ultra Pure — Use nitric acid
specified for ultra low metal ion content.
8.7.3.2 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.
8.7.4 Sample Preparation
8.7.4.1 In a clean environment, place 250 g 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.
Cool, and transfer quantitatively to a 50 mL volumetric
flask using 2% nitric acid for rinsing and dilution to
volume. Run a reagent blank.
8.7.5 Analysis
8.7.5.1 Using the acid sample and reagent blank,
analyze group 1 elements by flame atomic absorption
spectroscopy and all other elements by plasma emission
spectroscopy.
9 Grade 2 Procedures
NOTE 3: Each laboratory is responsible for verifying the
validity of the method within its own operation.
9.1 Non-Metal Impurities — See Section 8, which
contains procedures for the following tests:
Assay
Color (APHA)
Chloride
Phosphate
Sulfate
9.2 Trace Metals Analysis
9.2.1 The following method has given satisfactory
results in determining metal ion impurities at the values
specified for each of the following metals: aluminum
(Al), antimony (Sb), arsenic (As), barium (Ba),
beryllium (Be), bismuth (Bi), boron (B), calcium (Ca),
chromium (Cr), cobalt (Co), copper (Cu), gallium (Ga),
germanium (Ge), gold (Au), iron (Fe), lead (Pb),
lithium (Li), magnesium (Mg), manganese (Mn),
molybdenum (Mo), nickel (Ni), niobium (Nb),
potassium (K), silver (Ag), sodium (Na), strontium (Sr),
tantalum (Ta), tin (Sn), titanium (Ti), vanadium (V),
zinc (Zn), and zirconium (Zr). Alternate methods may
be used as long as appropriate studies demonstrate a
recovery between 75 - 125% of a known sample spike
for half of the value of each specified element.
9.2.2 Special Reagents
9.2.2.1 Nitric Acid, Ultra Pure — Use nitric acid
specified for low metal ion content.
9.2.2.2 7.0% Nitric Acid Solution — Dilute 20 g of
ultrapure nitric acid to 200 g using water meeting the
criteria for Type E1.1 in ASTM D5127.
9.2.2.3 Water — The water used for all the dilution,
calibration and standards should meet at a minimum the
criteria for Type E1.1 in ASTM D5127 in regard to
cation analysis.
9.2.2.4 Indium Internal Standard — Make up a
indium internal standard solution to a concentration of
20 µg/mL (ppm) from a appropriate concentrated
indium standard solution.
NITRIC ACID SEMI C35-0301 © SEMI 1979, 20013
9.2.3 Sample Preparation
9.2.3.1 In a clean environment, place 2.00 g of sample
into a tared FEP bottle (30 mL), dilute with Type E1.1
water to a final weight of 20.0 g. Add 20 µL of the
indium internal standard solution. Run a reagent blank.
9.2.4 Analysis
9.2.4.1 Using the prepared solutions and blanks,
analyze sodium, potassium, calcium and iron by
graphite furnace atomic absorption (GFAA) and the
remaining elements by inductively coupled plasma
mass spectrometry (ICP/MS). For calibration, the
standards are made up with the 7.0% nitric acid solution
and the indium internal standard such that the final
concentration is 20 ng/g of indium.
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 Standardized test methods are being developed
for all parameters at the purity levels indicated. Until
standardized test methods are published, test
methodology shall be determined by user and producer.
The Process Chemical 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.
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 Nitric Acid
Previous SEMI Reference # C1.12-96 C7.6-95 C8.6-95
Grade 1 Grade 2 Tier B
(Specification) (Specification) (Guideline)
Assay (HNO
3
) 69.0–70.0% 69.0–70.0% 69.0–70.0%
Color (APHA) 10 max
(see NOTE 1)
10 max 10 max
Chloride (Cl) 0.08 ppm max 80 ppb max 50 ppb max
Phosphate (PO
4
) 0.2 ppm max 200 ppb max 50 ppb max
Sulfate (SO
4
) 0.5 ppm max 500 ppb max 50 ppb max
Aluminum (Al) 0.2 ppm max 5 ppb max 1 ppb max
Antimony (Sb) -- 5 ppb max --
Arsenic (As) -- 10 ppb max --
Arsenic and Antimony (as As) 0.005 ppm max -- 1 ppb max
Barium (Ba) -- 10 ppb max 1 ppb max
Beryllium (Be) -- 10 ppb max 1 ppb max
Bismuth (Bi) -- 10 ppb max 1 ppb max
Boron (B) 0.1 ppm max 10 ppb max 1 ppb max
Cadmium (Cd) -- 5 ppb max 1 ppb max
Calcium (Ca) 0.2 ppm max 10 ppb max 1 ppb max
Chromium (Cr) 0.1 ppm max 10 ppb max 1 ppb max
Cobalt (Co) -- 10 ppb max 1 ppb max
Copper (Cu) 0.05 ppm max 10 ppb max 1 ppb max
Gallium (Ga) -- 10 ppb max 1 ppb max
Germanium (Ge) -- 5 ppb max 1 ppb max
SEMI C35-0301 © SEMI 1979, 2001 NITRIC ACID4
Previous SEMI Reference # C1.12-96 C7.6-95 C8.6-95
Grade 1 Grade 2 Tier B
(Specification) (Specification) (Guideline)
Gold (Au) 0.3 ppm max 5 ppb max 1 ppb max
Iron (Fe) 0.2 ppm max 5 ppb max 1 ppb max
Lead (Pb) 0.1 ppm max 10 ppb max 1 ppb max
Lithium (Li) -- 5 ppb max 1 ppb max
Magnesium (Mg) 0.3 ppm max 10 ppb max 1 ppb max
Manganese (Mn) 0.2 ppm max 10 ppb max 1 ppb max
Molybdenum (Mo) -- 10 ppb max 1 ppb max
Nickel (Ni) 0.05 ppm max 10 ppb max 1 ppb max
Niobium (Nb) -- 10 ppb max 1 ppb max
Potassium (K) 0.3 ppm max 5 ppb max 1 ppb max
Silicon (Si) -- -- 1 ppb max
Silver (Ag) -- 10 ppb max 1 ppb max
Sodium (Na) 0.3 ppm max 5 ppb max 1 ppb max
Strontium (Sr) -- 10 ppb max 1 ppb max
Tantalum (Ta) -- 10 ppb max 1 ppb max
Thallium (Tl) -- 10 ppb max 1 ppb max
Tin (Sn) 0.3 ppm max 10 ppb max 1 ppb max
Titanium (Ti) 0.3 ppm max 10 ppb max 1 ppb max
Vanadium (V) -- 10 ppb max 1 ppb max
Zinc (Zn) 0.3 ppm max 10 ppb max 1 ppb max
Zirconium (Zr) -- 10 ppb max 1 ppb max
Particles in bottles:
size, #/mL
≥ 1.0 µm, 25 max ≥ 0.5 µm, 25 max ≥ 0.5 µm, 5 max
≥ 0.2 µm, TBD
NOTE 1: This material may darken during storage due to a photochemical reaction.
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 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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