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4.9% H YDROFLUORIC ACID SEMI C29-0301 © SEMI 1990, 2001 3 the in dium internal standard solutio n. Run a reagent bla nk. 10.2.4 Anal ysis 10.2.4.1 Us ing the prepared solutions a n d b lanks, analyze s odium, potass ium,…
SEMI C29-0301 © SEMI 1990, 2001 4.9% HYDROFLUORIC ACID2
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 Hydrofluoric Acid, Ultra Pure — Use hydro-
fluoric acid specified for low metal ion content.
9.2.2.2 4.9% Hydrofluoric Acid Solution — Dilute 20
g of ultrapure hydrofluoric 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 the
internal standard solution to a concentration of 20
µg/mL (ppm) from the appropriate concentrated indium
standard solution.
9.2.3 Sample Preparation
9.2.3.1 In a clean environment, place 20.0 g of sample
into a tared FEP bottle (30 mL). 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 4.9% hydrofluoric acid
solution and a final concentration of 20 ng/g of the
indium internal standard.
NOTE 3: Analysis of diluted hydrofluoric acid requires the
use of special hydrofluoric acid resistant sample introduction
systems for inductively coupled plasma mass spectrometry.
These systems are available from most instrument suppliers.
NOTE 4: Analysis of diluted hydrofluoric acid can produce
rapid corrosion of nickel cones commonly used in inductively
coupled plasma mass spectrometry, platinum cones should be
considered as alternative when performing this analysis.
10 Grade 3 Procedures
NOTE 5: The analytical procedures associated with this
standard are not intended to be the only acceptable procedure
or the best procedure available. The published procedures
have been found to meet the required criteria for acceptance
of an analytical procedure. Alternate procedures may be used
if they meet the same criteria as the published procedures.
NOTE 6: Each laboratory is responsible for verifying the
validity of each method within its own operation.
10.1 Non-Metal Impurities — See SEMI C28, which
contains procedures for the following tests:
Assay
Color (APHA)
Fluosilicic Acid
Chlorides
Phosphates
Sulfate and Sulfite (as SO
4
)
10.1.1 Analysis of Anions and Fluosilicic Acid —
Application of the procedures cited above to dilute
hydrofluoric acid requires a tenfold increase in the
amount of inital sample weight prior to the evaporation
steps given in the procedures.
10.2 Trace Metals Analysis
10.2.1 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), boron
(B), cadmium (Cd), calcium (Ca), chromium (Cr),
cobalt (Co), copper (Cu), gold (Au), iron (Fe), lead
(Pb), lithium (Li), magnesium (Mg), manganese (Mn),
molybdenum (Mo), nickel (Ni), potassium (K), silver
(Ag), sodium (Na), strontium (Sr), tin (Sn), titanium
(Ti), vanadium (V), and zinc (Zn). 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.
10.2.2 Special Reagents
10.2.2.1 Hydrofluoric Acid, Ultrapure — Use hydro-
fluoric acid specified for low metal ion content.
10.2.2.2 4.9% Hydrofluoric Acid Solution — Dilute 20
g of ultrapure hydrofluoric acid to 200 g using water
meeting the criteria for Type E1.1 in ASTM D5127.
10.2.2.3 Water — The water used for all the dilution,
calibration, and standards should meet at a minimum
the criteria for Type E1.1 in ASTM D5127in regard to
cation analysis.
10.2.2.4 Indium Internal Standard — Make up the
internal standard solution to a concentration of 20
µg/mL (ppm) from the appropriate concentrated indium
standard solution.
10.2.3 Sample Preparation
10.2.3.1 In a clean environment, place 20.0 g of
sample into a tared FEP bottle (30 mL). Add 20 µL of
4.9% HYDROFLUORIC ACID SEMI C29-0301 © SEMI 1990, 20013
the indium internal standard solution. Run a reagent
blank.
10.2.4 Analysis
10.2.4.1 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 4.9% hydrofluoric acid
solution and a final concentration of 20 ng/g of the
indium internal standard.
NOTE 7: Analysis of dilute hydrofluoric acid requires the use
of special hydrofluoric acid-resistant sample introduction
systems for inductively coupled plasma mass spectrometry.
These systems are available from most instrument suppliers.
NOTE 8: Analysis of dilute hydrofluoric acid can produce
rapid corrosion of nickel cones commonly used in inductively
coupled plasma mass spectrometry; platinum cones should be
considered as an alternative when performing this analysis.
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 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 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.
17 Tier D Procedures
17.1 This section does not apply to this chemical.
Table 1 Impurity Limits and Other Requirements for 4.9% Hydrofluoric Acid
Previous SEMI Reference # C7.4-93 C8.4-0298 C12.3-96
Grade 2 Grade 3 Tier C
(Specification) (Specification) (Guideline)
Assay (HF) 4.8–5.0 % 4.8–5.0% 4.8–5.0%
Color (APHA) 10 max 10 max 10 max
Fluosilicic Acid (H
2
SiF
6
) 10 ppm max 10,000 ppb max 10,000 ppb max
Total Organic Carbon (TOC) -- -- 500 ppb max
Chloride (Cl) 500 ppb max 500 ppb max 100 ppb max
Phosphate (PO
4
) 100 ppb max 100 ppb max 100 ppb max
Sulfate (SO
4
) -- -- 100 ppb max
Sulfate and Sulfite (as SO
4
) 500 ppb max 500 ppb max --
Aluminum (Al) 10 ppb max 1 ppb max 100 ppt max
Antimony (Sb) -- 1 ppb max 100 ppt max
Arsenic (As) -- 1 ppb max 100 ppt max
Arsenic and Antimony (as As) 5 ppb max -- --
Barium (Ba) 10 ppb max 1 ppb max --
Beryllium (Be) 5 ppb max -- --
Bismuth (Bi) 5 ppb max -- --
Boron (B) 10 ppb max 1 ppb max 100 ppt max
Cadmium (Cd) 10 ppb max 1 ppb max --
Calcium (Ca) 10 ppb max 1 ppb max 100 ppt max
Chromium (Cr) 10 ppb max 1 ppb max 100 ppt max
Cobalt (Co) 10 ppb max 1 ppb max --
SEMI C29-0301 © SEMI 1990, 2001 4.9% HYDROFLUORIC ACID4
Previous SEMI Reference # C7.4-93 C8.4-0298 C12.3-96
Grade 2 Grade 3 Tier C
(Specification) (Specification) (Guideline)
Copper (Cu) 10 ppb max 1 ppb max 100 ppt max
Gallium (Ga) 10 ppb max -- --
Germanium (Ge) 10 ppb max -- --
Gold (Au) 5 ppb max 1 ppb max 100 ppt max
Iron (Fe) 10 ppb max 1 ppb max 100 ppt max
Lead (Pb) 10 ppb max 1 ppb max 100 ppt max
Lithium (Li) 5 ppb max 1 ppb max --
Magnesium (Mg) 10 ppb max 1 ppb max 100 ppt max
Manganese (Mn) 10 ppb max 1 ppb max 100 ppt max
Molybdenum (Mo) 10 ppb max 1 ppb max --
Nickel (Ni) 10 ppb max 1 ppb max 100 ppt max
Niobium (Nb) 10 ppb max -- --
Potassium (K) 10 ppb max 1 ppb max 100 ppt max
Silver (Ag) 5 ppb max 1 ppb max --
Sodium (Na) 10 ppb max 1 ppb max 100 ppt max
Strontium (Sr) 10 ppb max 1 ppb max --
Tantalum (Ta) 10 ppb max -- --
Thallium (Tl) 10 ppb max -- --
Tin (Sn) 10 ppb max 1 ppb max 100 ppt max
Titanium (Ti) 10 ppb max 1 ppb max 100 ppt max
Vanadium (V) 10 ppb max 1 ppb max --
Zinc (Zn) 10 ppb max 1 ppb max 100 ppt max
Zirconium (Zr) 10 ppb max -- --
Particles in bottles:
size, #/mL
≥ 0.5 µm, 25 max ≥ 0.5 µm, 25 max ≥ 0.2 µm, TBD
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