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SEMI C27-0301 © SEMI 1978, 2001 HYDROCH LORIC ACID 4 Recovery i s for a kno wn sample spike at 50% of th e specified level. 16 Tier C P rocedures 16.1 S tandardized test methods are b e i ng developed for all p arameters…
HYDROCHLORIC ACID SEMI C27-0301 © SEMI 1978, 20013
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 Section 8, which
contains procedures for the following tests:
Assay
Color (APHA)
Free Halogen
Phosphate
Sulfate
Sulfite
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 Hydrochloric Acid, Ultrapure — Use
hydrochloric acid specified for low metal ion content.
9.2.2.2 3.7% Hydrochloric Acid Solution — Dilute 20
g of ultrapure hydrochloric acid to 200 g using water
meeting the criteria for Type E1.1 in ASTM D5127.
9.2.2.3 Nitric Acid, Ultrapure — Use nitric acid
specified for low metal ion content.
9.2.2.4 1% Nitric Acid Solution — Dilute 10 mL of
ultrapure nitric acid to 1 L using water meeting the
criteria for Type E1.1 in ASTM D5127.
9.2.2.5 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.
9.2.2.6 Rhodium Internal Standard — Make up the
internal standard solution to a concentration of 20
µg/mL (ppm) from the appropriate concentrated
standard rhodium solution.
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 “attainable”
water to a final weight of 20.0 g. Add 20 µL of the
rhodium internal standard solution. Run a reagent
blank.
9.2.3.2 Vanadium — In a clean environment, place
20.0 g of sample into a clean PTFE dish. Slowly
evaporate on a hot plate to dryness avoiding loss of
sample by effervescence or spattering. Dissolve the
residue with 5 mL of the 1% nitric acid solution by
heating on a hot plate at low temperature for several
minutes. Cool to room temperature, dilute to 20 g with
1% nitric acid, add 20 µL of the rhodium internal
standard, mix well. 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 3.7% hydrochloric acid
solution and the rhodium internal standard except for
the analysis of vanadium which is performed using 1%
nitric acid as the matrix. All standards must contain 10
ng/g of rhodium as the internal standard.
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 Sections 8 and 9 for available procedures.
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 supplier.
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%.
SEMI C27-0301 © SEMI 1978, 2001 HYDROCHLORIC ACID4
Recovery is for a known sample spike at 50% of the
specified level.
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 Hydrochloric Acid
Previous SEMI Reference # C1.7-95 C7.2-94 C11.6-1296 C8.2-92 C12.2-96
Grade 1 Grade 2 VLSI Grade Tier B Tier C
(Specification) (Specification) (Guideline) (Guideline) (Guideline)
Assay (HCl) 36.5–38.0% 36.5–38.0 % 36–38% 37.0–38.0% 37.0–38.0%
Color (APHA) 10 max 10 max 10 max 10 max 10 max
Extractable Organic Substances 5 ppm max -- -- 500 ppb max --
Residue after Ignition (as SO
4
) -- -- 3 ppm max -- --
Free Halogen (as Cl
2
) To pass test To pass test -- 500 ppb max 500 ppb max
Free Chlorine (Cl
2
) -- -- 0.5 ppm max -- --
Bromide (Br) -- -- 50 ppm max -- --
Phosphate (PO
4
) 0.05 ppm max 50 ppb max 0.05 ppm max 50 ppb max 50 ppb max
Sulfate (SO
4
) 0.5 ppm max 500 ppb max 0.5 ppm max 100 ppb max 30 ppb max
Sulfite (SO
3
) 0.8 ppm max 800 ppb max 0.7 ppm max 100 ppb max 100 ppb max
Aluminum (Al) 0.3 ppm max 10 ppb max 0.05 ppm max 1 ppb max 100 ppt max
Antimony (Sb) -- 5 ppb max 0.005 ppm max -- 100 ppt max
Arsenic (As) -- 10 ppb max 0.005 ppm max -- 100 ppt max
Arsenic and Antimony (as As) 0.005 ppm max -- -- 1 ppb max --
Barium (Ba) -- 10 ppb max 0.05 ppm max 1 ppb max 100 ppt max
Beryllium (Be) -- 10 ppb max 0.02 ppm max 1 ppb max --
Bismuth (Bi) -- 10 ppb max 0.02 ppm max 1 ppb max --
Boron (B) 0.1 ppm max 10 ppb max 0.02 ppm max 1 ppb max 100 ppt max
Cadmium (Cd) -- 10 ppb max 0.005 ppm max 1 ppb max --
Calcium (Ca) 0.3 ppm max 10 ppb max 0.2 ppm max 1 ppb max 100 ppt max
Chromium (Cr) 0.2 ppm max 10 ppb max 0.01 ppm max 1 ppb max 100 ppt max
Cobalt (Co) -- 10 ppb max 0.01 ppm max 1 ppb max 100 ppt max
Copper (Cu) 0.1 ppm max 10 ppb max 0.01 ppm max 1 ppb max 100 ppt max
Gallium (Ga) -- 10 ppb max 0.02 ppm max 1 ppb max --
Germanium (Ge) -- 10 ppb max -- 1 ppb max --
Gold (Au) 0.3 ppm max 5 ppb max 0.02 ppm max 1 ppb max --
Indium (In) -- -- 0.02 ppm max -- --
Iron (Fe) 0.2 ppm max 10 ppb max 0.1 ppm max 1 ppb max 100 ppt max
Lead (Pb) 0.1 ppm max 10 ppb max 0.02 ppm max 1 ppb max 100 ppt max
Lithium (Li) -- 10 ppb max 0.02 ppm max 1 ppb max --
Magnesium (Mg) 0.3 ppm max 10 ppb max 0.05 ppm max 1 ppb max 100 ppt max
Manganese (Mn) 0.3 ppm max 10 ppb max 0.01 ppm max 1 ppb max 100 ppt max
Mercury (Hg) -- -- 0.02 ppm max -- --
Molybdenum (Mo) -- 10 ppb max 0.02 ppm max 1 ppb max --
Nickel (Ni) 0.1 ppm max 10 ppb max 0.01 ppm max 1 ppb max 100 ppt max
Niobium (Nb) -- 10 ppb max -- 1 ppb max --
HYDROCHLORIC ACID SEMI C27-0301 © SEMI 1978, 20015
Previous SEMI Reference # C1.7-95 C7.2-94 C11.6-1296 C8.2-92 C12.2-96
Grade 1 Grade 2 VLSI Grade Tier B Tier C
(Specification) (Specification) (Guideline) (Guideline) (Guideline)
Platinum (Pt) -- -- 0.02 ppm max -- --
Potassium (K) 0.3 ppm max 10 ppb max 0.05 ppm max 1 ppb max 100 ppt max
Silicon (Si) -- -- -- 1 ppb max --
Silver (Ag) -- 5 ppb max 0.02 ppm max 1 ppb max --
Sodium (Na) 0.3 ppm max 10 ppb max 0.1 ppm max 1 ppb max 100 ppt max
Strontium (Sr) -- 10 ppb max 0.02 ppm max 1 ppb max --
Tantalum (Ta) -- 10 ppb max -- 1 ppb max 100 ppt max
Thallium (Tl) -- 10 ppb max 0.02 ppm max 1 ppb max --
Tin (Sn) 0.3 ppm max 10 ppb max 0.02 ppm max 1 ppb max 100 ppt max
Titanium (Ti) 0.3 ppm max 10 ppb max 0.05 ppm max 1 ppb max 100 ppt max
Vanadium (V) -- 10 ppb max 0.02 ppm max 1 ppb max --
Zinc (Zn) 0.3 ppm max 10 ppb max 0.05 ppm max 1 ppb max 100 ppt max
Zirconium (Zr) -- 10 ppb max 0.02 ppm max 1 ppb max --
Particles in bottles
(size, #/mL)
≥ 1.0 µm, 25 max ≥ 0.5 µm, 25 max ≥ 0.5 µm, 250 max ≥ 0.5 µm, 10 max
≥ 0.2 µm, TBD
(See NOTE 1.)
NOTE 1: 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.
Table 2 Composition of Standard
Substance Amount in 500 mL of 2,2,4-trimethylpentane
solution
Concentration in ppm for 5 mL of standard in 100
mL (120 g) of HCl
µL
mg
Benzene 6.8 6 0.5
Chlorobenzene 5.5 6 0.5
1,2-Dichloroethane 20 25 2.0
Chloroform 34 50 4.0
DDT (see NOTE 1) 25 2.0
Total 9.0
Allowance for CCl
4
1.0
Total 10.0
NOTE 1: 1,1,1-Trichloro-2,2-bis (p-chlorophenyl) ethane, dichlorodiphenyltrichloroethane.
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