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4.9% H YDROFLUORIC ACID SEMI C29-0301 © SEMI 1990, 2001 1 SEMI C29-0301 SPECIFICA TIONS AND GUIDELINE FOR 4.9% HY DROFLUORIC ACID (10:1 v/v ) These speci fications an d this gu ideline were techn ically ap proved by th e…
HYDROFLUORIC ACID SEMI C28-0705 © SEMI 1978, 2005 5
16 Tier D Procedures
16.1 This section does not apply to this chemical.
Table 1 Impurity Limits and Other Requirements for Hydrofluoric Acid
Previous SEMI Reference # C1.8-95 C7.3-93 C8.3-96 -
Grade 1 Grade 2 Grade 3 Grade 4
(Specification) (Specification) (Specification)
(Specification)
Assay (HF) 48.8–49.2% 48.8–49.2 % 48.90–49.10% 48.90–49.10%
Appearance Clear and colorless Clear and colorless Clear and colorless Clear and colorless
Chloride (Cl) 5 ppm max 5000 ppb max 200 ppb max 100 ppb max
Nitrate (NO
3
) 3 ppm max 3000 ppb max 100 ppb max 100 ppb max
Phosphate (PO
4
) 1 ppm max 1000 ppb max 100 ppb max 100 ppb max
Sulfate (SO
4
) -- -- 200 ppb max 100 ppb max
Sulfate and Sulfite (as SO
4
) 5 ppm max 5000 ppb max --
Aluminum (Al) 0.05 ppm max 10. ppb max 1 ppb max 100 ppt max
Antimony (Sb) 0.03 ppm max 15 ppb max 1 ppb max 100 ppt max
Arsenic (As) 0.03 ppm max 15 ppb max 1 ppb max 100 ppt max
Barium (Ba) -- 10. ppb max 1 ppb max 100 ppt max
Boron (B) 0.05 ppm max 10. ppb max 1 ppb max 100 ppt max
Cadmium (Cd) -- 10. ppb max 1 ppb max 100 ppt max
Calcium (Ca) 0.3 ppm max 10. ppb max 1 ppb max 100 ppt max
Chromium (Cr) 0.01 ppm max 10. ppb max 1 ppb max 100 ppt max
Copper (Cu) 0.05 ppm max 10. ppb max 1 ppb max 100 ppt max
Iron (Fe) 0.2 ppm max 10. ppb max 1 ppb max 100 ppt max
Lead (Pb) 0.1 ppm max 10. ppb max 1 ppb max 100 ppt max
Lithium (Li) -- 5. ppb max 1 ppb max 100 ppt max
Magnesium (Mg) 0.2 ppm max 10. ppb max 1 ppb max 100 ppt max
Manganese (Mn) 0.2 ppm max 10. ppb max 1 ppb max 100 ppt max
Nickel (Ni) 0.1 ppm max 10. ppb max 1 ppb max 100 ppt max
Potassium (K) 0.3 ppm max 10. ppb max 1 ppb max 100 ppt max
Sodium (Na) 0.3 ppm max 10. ppb max 1 ppb max 100 ppt max
Tin (Sn) 0.3 ppm max 10. ppb max 1 ppb max 100 ppt max
Titanium (Ti) 0.3 ppm max 10. ppb max 1 ppb max 100 ppt max
Vanadium (V) -- 10. ppb max 1 ppb max 100 ppt max
Zinc (Zn) 0.3 ppm max 10. ppb max 1 ppb max 100 ppt max
Particles in bottles
(size, #/mL)
1.0 m, 25 max 0.5 m, 25 max 0.5 m, 5 max
0.2 m, TBD
TBD
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4.9% HYDROFLUORIC ACID SEMI C29-0301 © SEMI 1990, 20011
SEMI C29-0301
SPECIFICATIONS AND GUIDELINE FOR 4.9% HYDROFLUORIC ACID
(10:1 v/v)
These specifications and this guideline 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 C7.4,
C8.4, and C12.3 in their entirety. Originally published in 1990, 1992, and 1995 respectively; previously
published June 1999.
1 Purpose
1.1 The purpose of this document is to standardize
requirements for 4.9% hydrofluoric 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 4.9% hydrofluoric
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 4.9%
hydrofluoric acid used in the semiconductor industry.
2.2 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.
3 Limitations
3.1 None.
4 Referenced Standards
4.1 SEMI Standards
SEMI C28 — Specifications and Guidelines for
Hydrofluoric Acid
4.2 ASTM Standards
1
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.
5 Terminology
5.1 None.
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
6 Physical Property (for information only)
6.1 Not applicable.
7 Requirements
7.1 The requirements for 4.9% hydrofluoric acid for
Grades 2 and 3 and Tier C are listed in Table 1.
8 Grade 1 Procedures
8.1 This section does not apply to this chemical.
9 Grade 2 Procedures
NOTE 2: Each laboratory is responsible for verifying the
validity of the method within its own operation.
9.1 Non-Metal Impurities — See SEMI C28
(Specifications and Guidelines for Hydrofluoric Acid)
which contains procedures for the following tests:
Assay
Color (APHA)
Fluosilicic Acid
Chloride
Phosphate
Sulfate and Sulfite (as SO
4
)
Arsenic and Antimony (as As)
9.1.1 Analysis of Anions and Fluosilicic Acid —
Application of the procedures cited above to dilute
hydrofluoric acid requires a tenfold increase in the
amount of initial sample weight prior to the evaporation
steps given in the procedures.
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), arsenic (As), antimony (Sb), 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),
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