semi合集-English.pdf - 第6652页

HYDROCHLORIC ACID SEM I C27-0301 © SEMI 1978, 2001 3 9 Grade 2 P rocedu res NOTE 2: Ea ch laborat ory is res ponsible for verify ing the validity of the me thod within i ts own oper ation. 9.1 Non-Metal Impurities — See …

100%1 / 7923
SEMI C27-0301 © SEMI 1978, 2001 HYDROCHLORIC ACID2
Chromosorb P (80/100), 3 m × 3 mm stainless steel or
glass; injection port at 280°C with glass insert; column
temperature initially 65°C, programmed at 6°C/min up
to 140°C; carrier gas — nitrogen at 40 mL/min; signal
adjusted to give an 80% full-scale deflection; and
preferably, electronic integration of peak areas. For
DDT: Column — 5% silicone gum SESE-30 on
Chromosorb W (60/80), 1.5 × 3 mm, injection port —
as above; column temperature — isothermal at 205°C;
carrier gas — nitrogen at 75 mL/min, and preferably,
electronic integration of peak areas. The order of
elution is 2,2,4-trimethylpentane, carbon tetrachloride,
benzene, chloroform, 2,2,4-trimethylpentane impurity,
1,2-dichloroethane, chlorobenzene, and dichloro-
benzene. The total area under the impurity peaks from
the sample should be no greater than that from the
blank (extract from second funnel) by more than one-
half the total area under the peaks from the standard
(third funnel), also corrected for the blank.
8.3.1 Standard — Use a syringe to add the volumes of
liquid listed in Table 2 into 300 mL of 2,2,4-
trimethylpentane. Add 25 mg of DDT to the solution.
Dilute to 500 mL with 2,2,4-trimethylpentane. The
2,2,4-trimethylpentane used for both the standard and
the analysis should be free from impurities that interfere
with the chromatographic analysis.
8.4 Free Halogen (as Cl
2
) — Mix 100 mL of sample
and 100 mL of freshly boiled water and cool. Add 0.1
mL of 2% potassium iodide reagent solution and 1 mL
of carbon disulfide, and mix. The carbon disulfide
should not acquire a pink color in one-half minute.
8.5 Phosphate — To 170 mL (200 g) of sample, add
10 mL of sodium carbonate reagent solution and
evaporate to dryness on a steam bath in a hood.
Dissolve the residue in 25 mL of 0.5 N sulfuric acid.
Add 1 mL of ammonium molybdate reagent solution
and 1 mL of p-(methylamino)phenol solution. Allow to
stand at room temperature for 2 hours. Any blue color
produced should be no greater than that produced when
0.01 mg of phosphate ion (PO
4
) is treated like the
sample.
8.6 Sulfate — To 84 mL (100 g) of sample, add 10 mL
of sodium carbonate reagent solution and evaporate to
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 10 minutes.
Any turbidity should be no greater than that produced
when 0.05 mg of sulfate ion (SO
4
) is treated as the
sample.
8.7 Sulfite — Add 1 mL of 10 percent potassium
iodide reagent solution, 5 mL of hydrochloric acid, and
2 mL of starch indicator solution to 400 mL of oxygen-
free water. Add 0.01 N iodine until a faint permanent
blue color is produced. Add 85 mL of the sample and
titrate with 0.01 N iodine to the same endpoint. Not
more than 0.20 mL should be required.
8.8 Arsenic and Antimony (as As) — To 168 mL (200
g) of sample in a 400 mL beaker, add 10 mL of nitric
acid and 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 tile sentence which begins: “Swirl the flask....”
Any red color in the silver diethyldithiocarbamate
solution from the sample should be no greater than that
of the standard containing 0.001 mg of arsenic (As).
8.9 Trace Metal Analysis — The following method
has given satisfactory results in determing trace metal
impurities at the value specified for each of the
following trace metals: aluminum (Al), boron (B),
calcium (Ca), chromium (Cr), copper (Cu), gold (Au),
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.
8.9.1 Special Reagents
8.9.1.1 Nitric Acid, Ultra Pure — Use nitric acid
specified for ultra low metal ion content.
8.9.1.2 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.
8.9.2 Sample Preparation
8.9.2.1 In a clean environment, place 250 mL 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. Note: Evaporation typically requires 2 1/2 to 4
hours. Cool. Transfer quantitatively to a 50 mL
volumetric flask using 2% nitric acid for rinsing and
dilution to volume. Run a reagent blank.
8.9.3 Analysis
8.9.3.1 Using the acid sample and reagent blank,
analyze group 1 elements by flame atomic absorption
spectroscopy and all other elements by plasma emission
spectroscopy.
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 --