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SEMI C28-0705 © SEMI 1997, 2005 HYDROFL UORIC ACID 4 by the method of standard a ddition. Alternate method can be used as long as method validation according to SEM I C1 can be demonstrated. 10.3 Trace Metal Analysis — T…

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HYDROFLUORIC ACID SEMI C28-0705 © SEMI 1978, 2005 3
8.6.3 Analysis
8.6.3.1 Using the acid sample and reagent blank, analyze all specified elements by plasma emission spectroscopy or
preferably by ICP-MS.
9 Grade 2 Procedures
NOTE 4: Each laboratory is responsible for verifying the validity of the method within its own operation.
9.1 Non-Metal Impurities — See §8, which contains procedures for the following tests:
Assay,
Chloride,
Nitrate,
Phosphate, and
Sulfate and Sulfite (as SO
4
).
9.2 Trace Metals Analysis
9.2.1 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), antimony (Sb), arsenic (As), barium (Ba), boron
(B), cadmium (Cd), calcium (Ca), chromium (Cr), copper (Cu), iron (Fe), lead (Pb), lithium (Li), magnesium (Mg),
manganese (Mn), nickel (Ni), potassium (K), sodium (Na), tin (Sn), titanium (Ti), vanadium (V), and zinc (Zn).
Alternate method can be used as long as method validation according to SEMI C1 can be demonstrated.
9.2.2 Special Reagents
9.2.2.1 Hydrofluoric Acid, Ultra Pure — Use hydrofluoric 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 a internal standard solution to a concentration of 20 g/mL (ppm)
from the appropriate concentrated indium standard solution.
9.2.3 Sample Preparation — 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 L 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 all the specified elements by inductively coupled plasma
mass spectrometry (ICP/MS). For calibration, the standards are made up with the 4.9% hydrofluoric acid solution
and the indium internal standard such that the final concentration is 20 ng/g of indium.
NOTE 5: 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 6: 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 alternative when performing this analysis.
10 Grade 3 Procedures
10.1 Assay — See ¶8.1
10.2 Chloride, Nitrate, Sulfate, Phosphate
10.2.1 The above mentioned anions can be determined by ion chromatography using a two dimensional approach.
For a detailed procedure, see for example Dionex Technical Note 45. Better results are obtained when using an
IonPac ICE-AS1 column instead of the IonPac ICE-AS6 recommended in the TN45. Calibration is preferably done
SEMI C28-0705 © SEMI 1997, 2005 HYDROFLUORIC ACID 4
by the method of standard addition. Alternate method can be used as long as method validation according to SEMI
C1 can be demonstrated.
10.3 Trace Metal Analysis — 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), antimony (Sb), arsenic (As),
barium (Ba), boron (B), cadmium (Cd), calcium (Ca), chromium (Cr), copper (Cu), iron (Fe), lead (Pb), lithium (Li),
magnesium (Mg), manganese (Mn), nickel (Ni), potassium (K), sodium (Na), tin (Sn), titanium (Ti), vanadium (V),
and zinc (Zn). Alternate method can be used as long as method validation according to SEMI C1 can be
demonstrated.
10.3.1 Special Reagents
10.3.1.1 Nitric Acid, Ultra Pure — Use nitric acid specified for ultra low metal ion content.
10.3.1.2 3 % Nitric Acid Solution — In a clean environment, place 15 g of Ultra Pure Nitric Acid ¶10.3.1.1 into a
tared clean 500 ml FEP bottle. Dilute to a final weight of 500 g using ultrapure water ¶10.3.1.3.
10.3.1.3 Water — The water used for all the dilutions, calibrations and standards should meet at a minimum the
criteria for Type E1.2 in ASTM D5127 in regard to cation analysis.
10.3.2 Sample Preparation
10.3.2.1 In a clean environment, place 20 g of sample into a tared clean 120 ml FEP bottle. Dilute to a final weight
of 100 g with the 3 % Nitric Acid Solution ¶10.3.1.2.
10.3.3 Analysis
10.3.3.1 Using the prepared solutions, analyze all the specified elements by inductively coupled plasma mass
spectrometry (ICP-MS). For calibration, blank and standards are made up with the 3 % Nitric Acid Solution
¶10.3.1.2.
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 alternative when performing this analysis.
NOTE 9: The analytical methodology described in ¶10.3 has been validated using a “Reaction / Collision cell” type ICP-MS.
Other instrument type can be used as long as method validation according to SEMI C1 can be demonstrated.
11 Grade 4 Procedures
11.1 Assay — See ¶8.1.
11.2 Chloride, Nitrate, Sulfate, Phosphate — See ¶10.2.
11.3 Trace Metal Analysis — See ¶10.3.
12 Grade 5 Procedures
12.1 This section does not apply to this chemical.
13 Tier A Procedures
13.1 This section does not apply to this chemical.
14 Tier B Procedures
14.1 This section does not apply to this chemical
15 Tier C Procedures
15.1 This section does not apply to this chemical
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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