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SEMI C33-0301 © SEMI 1986, 2001 n-METHYL 2-PYRROLIDONE 4 tin (Sn), titan ium (Ti), vanadium (V), an d zinc (Zn). Alte rnate methods may be u sed as long as appropriate studi es demonstrat e a recovery between 75 - 125% o…

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n-METHYL 2-PYRROLIDONE SEMI C33-0301 © SEMI 1986, 20013
8.8.2 Sample Preparation
8.8.2.1 In a clean environment, place 250 g of solvent
in a PTFE dish. Add 0.5 mL of freshly prepared 5%
mannitol solution. Slowly evaporate on a hot plate,
avoiding loss of sample by effervescence or spattering
until approximately 1 mL of liquid remains. Take up
liquid and all visible residue (from walls of dish) with 1
mL ultra pure, 12 M hydrochloric acid and continue
heating until approximately 0.5 mL of liquid remains.
No undissolved particulate matter should be observed.
Otherwise, repeat the addition of hydrochloric acid until
all particulate matter is dissolved. Transfer
quantitatively to a 50 mL volumetric flask using 2%
(v/v) hydrochloric acid and adjust liquid level to mark.
Prepare a reagent blank using the same reagents and in
the same manner as for the sample concentration.
8.8.3 Analysis
8.8.3.1 Using the prepared sample and reagent blank,
analyze group 1 elements potassium (K) and sodium
(Na) by atomic absorption spectroscopy and all other
elements by plasma emission spectrometry. Apply, if
necessary, a reagent blank correction to the final
determined value of the sample.
9 Grade 2 Procedures
9.1 Non-Metal Impurities — See Section 8, which
contains procedures for the following tests:
Assay
Color (APHA)
Water (H
2
O)
9.2 Methyl Amines
9.2.1 The following method has given satisfactory
results in determining methyl amine impurities at the
values specified for each of the following methyl
amines: mono-methylamine (MMA), di-methylamine
(DMA), and tri-methylamine (TMA). Alternative
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 Eluent — Prepare 0.025 N hydrochloric (HCl)
solution in deionized water meeting the criteria for
Type E1.1 in ASTM D5127.
9.2.2.2 Regenerant — Prepare a 0.1 M tetrabutyl-
ammonium hydroxide (TBAOH) solution in deionized
water meeting the criteria for Type E1.1 in ASTM
D5127.
9.2.3 Sample Preparation — Sample is injected neat.
9.2.4 Analysis
9.2.4.1 Using the prepared solutions and blanks,
analyze mono-methylamine, di-methylamine, and tri-
methylamine by ion chromatography. Run a reagent
blank. Samples and reagent blanks should be prepared
and analyzed in triplicate.
9.2.4.2 Columns — Precolumn should be CG2
(Dionex) or equivalent and separation column should
be a CS2 (Dionex) or equivalent.
9.3 Anions
9.3.1 The following method has given satisfactory
results in determining various anions at the values
specified for each of the following anions: chloride
(Cl), nitrate (NO
3
), phosphate (PO
4
), and sulfate (SO
4
).
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 anion.
9.3.2 Special Reagents
9.3.2.1 Eluent — Prepare a solution containing 0.38 g
of sodium carbonate (Na
2
CO
3
) and 0.29 g of sodium
bicarbonate (NaHCO
3
) in 2 liters of deionized water
meeting the criteria for Type E1.1 in ASTM D5127.
9.3.2.2 Regenerant — Deionized water meeting the
criteria for Type E1.1 in ASTM D5127.
9.3.3 Sample Preparation
9.3.3.1 20 mL of NMP is added to a 100 mL plastic
volumetric flask and is filled to the mark using
deionized water meeting the criteria for Type E1.1 in
ASTM D5127.
9.4 Analysis
9.4.1 Using the prepared solutions and blanks, analyze
chloride, nitrate, phosphate, and sulfate by ion
chromatography. Run a reagent blank. Samples and
blanks should be prepared in triplicate.
9.4.2 Columns — Precolumn should be AG3 (Dionex)
or equivalent and the separation column should be AS3
(Dionex) or equivalent.
9.5 Trace Metals Analysis
9.5.1 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), boron (B), cadmium
(Cd), calcium (Ca), chromium (Cr), cobalt (Co), copper
(Cu), gold (Au), iron (Fe), lead (Pb), lithium (Li),
magnesium (Mg), manganese (Mn), nickel (Ni),
potassium (K), silver (Ag), sodium (Na), strontium (Sr),
SEMI C33-0301 © SEMI 1986, 2001 n-METHYL 2-PYRROLIDONE4
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.
9.5.2 Special Reagents
9.5.2.1 Nitric Acid, Ultra Pure — Use nitric acid
specified for low metal ion content.
9.5.2.2 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.
9.5.2.3 Indium Internal Standard — Make up the
indium internal standard solution to a concentration of
20 µg/mL (ppm) from the appropriate concentrated
indium standard solution.
9.5.3 Sample Preparation
9.5.3.1 Place sample (1 gram) in a quartz dish. Slowly
evaporate to dryness (45 min. at 70–80°C). Add 2
grams of concentrated nitric acid and heat for 15 miutes
until approximately 1 gram remains. Remove the
hotplate and add DI water to a final weight of 10 grams.
9.5.4 Analysis
9.5.4.1 Using the prepared solution and blanks,
analyze the elements by inductively coupled plasma
mass spectrometry (ICP/MS). For calibration, the
standards are made up with 1% nitric acid solution and
the indium internal standard such that the final indium
concentration is 20 ng/g.
10 Grade 3 Procedures
10.1 Non-Metal Impurities — See Section 8, which
contains procedures for the following tests:
Assay
Color (APHA)
Water (H
2
O)
10.2 Methyl Amines
10.2.1 The following method has given satisfactory
results in determining methyl amine impurities at the
values specified for each of the following methyl
amines: mono-methylamine (MMA), dimethylamine
(DMA), and trimethylamine (TMA). Alternative
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 Eluent — Prepare 0.025 N hydrochloric acid
(HCl) solution in deionized water meeting the criteria
for Type E1.1 in ASTM D5127.
10.2.2.2 Regenerant — Prepare a 0.1 M tetrabutyl-
ammonium hydroxide (TBAOH) solution in deionized
water meeting the criteria for Type E1.1 in ASTM
D5127.
10.2.3 Sample Preparation — Sample is injected neat.
10.2.4 Analysis
10.2.4.1 Using the prepared solutions and blanks,
analyze mono-methylamine, di-methylamine, and tri-
methylamine by ion chromatography. Run a reagent
blank. Samples and reagent blanks should be prepared
and analyzed in triplicate.
10.2.4.2 Columns — Pre-column should be CG2
(Dionex) or equivalent and separation column should
be a CS2 (Dionex) or equivalent.
10.3 Anions
10.3.1 The following method has given satisfactory
results in determining various anions at the values
specified for each of the following anions: chloride
(Cl), nitrate (NO
3
) phosphate (PO
4
) and sulfate (SO
4
).
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 anion.
10.3.2 Special Reagents
10.3.2.1 Eluent — Prepare a solution containing 0.38
g of sodium carbonate (Na
2
CO
3
) and 0.29 g of sodium
bicarbonate (NaHCO
3
) in 2 liters of deionized water
meeting the criteria for Type E1.1 in ASTM D5127.
10.3.2.2 Regenerant — Deionized water meeting the
criteria for Type E1.1 in ASTM D5127.
10.3.3 Sample Preparation
10.3.3.1 20 mL of NMP is added to a 100 mL plastic
volumetric flask and is filled to the mark using
deionized water meeting the criteria for Type E1.1 in
ASTM D5127.
10.3.4 Analysis
10.3.4.1 Using the prepared solutions and blanks,
analyze chloride, nitrate, phosphate, and sulfate by ion
chromatography. Run a reagent blank. Samples and
blanks should be prepared in triplicate.
10.3.4.2 Columns — Pre-column should be AG3
(Dionex) or equivalent and the separation column
should be AS3 (Dionex) or equivalent.
n-METHYL 2-PYRROLIDONE SEMI C33-0301 © SEMI 1986, 20015
10.4 Trace Metal Analysis
10.4.1 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), 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 a recovery
between 75–125% of a known sample spike for half of
the value of each specified element.
10.4.2 Special Reagents
10.4.2.1 Nitric Acid, Ultra Pure — Use nitric acid
specified for low metal ion content.
10.4.2.2 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.
10.4.3 Sample Preparation
10.4.3.1 In a 100 mL volumetric, add 20 mL of sample
and fill to the mark such that the final solution contains
2% nitric acid.
10.4.4 Standard Preparation
10.4.4.1 Four standards are prepared such that the
final solution contains 2% nitric acid (i.e., 2% of 70%
nitric acid vol/vol) and 20% vol/vol sample. The four
standards are 0.5, 1, 5, and 10 ppb.
10.4.5 Analysis
10.4.5.1 This is a method of standard addition
procedure. Using the prepared solutions, analyze the
elements by inductively coupled plasma mass
spectrometry (ICP/MS).
10.4.5.2 Hot plasma conditions with shield are used
for the following elements: Ti, Mn, Ni, Cu, As, Sb, Sn,
Au, and Pb.
10.4.5.3 Cold plasma conditions with shield are used
for the follow elements, B, Na, Mg, Al, K, Ca, Cr, Fe,
and Zn.
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 This section does not apply to this chemical.
17 Tier D Procedures
17.1 This section does not apply to this chemical.
Table 1 Impurity Limits and Other Requirements for n-Methyl 2-Pyrrolidone
Previous SEMI Reference # C1.25-95 C7.16-95 C8.11-0698
Grade 1 Grade 2 Grade 3
(Specification) (Specification) (Specification)
Assay (see NOTE 1) (CH
3
N(CH
2
)
3
CO) 99.5% min 99.8% min 99.8%
Color (APHA) 50 max 50 max 30 max
Water (H
2
O) 0.05% max 0.05% max 0.03% max
Free Amines (as CH
3
NH
2
) 50 ppm max 5,000 ppb max 5 ppm max
Chloride (Cl) 1 ppm max 500 ppb max 300 ppb max
Nitrate (NO
3
) -- 500 ppb max 400 ppb max
Phosphate (PO
4
) 5 ppm max 500 ppb max 250 ppb max
Sulfate (SO
4
) -- 500 ppb max 250 ppb max
Aluminum (Al) 0.1 ppm max 20 ppb max 5 ppb max
Antimony (Sb) -- 20 ppb max 10 ppb max
Arsenic (As) -- 20 ppb max 10 ppb max
Arsenic and Antimony (as As) 0.1 ppm max -- --