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n-METHYL 2-PYRROLIDONE SEM I C33-0301 © SEMI 1 986, 2001 3 8.8.2 Sam ple Preparat ion 8.8.2.1 In a clean environment, place 2 5 0 g of solvent in a PTFE dis h. Add 0.5 mL of freshly prepared 5% mannitol solution. Slo wly…

100%1 / 7923
SEMI C33-0301 © SEMI 1986, 2001 n-METHYL 2-PYRROLIDONE2
8.3 Water — Add 25 mL of methanol to a dry titration
flask and add Karl Fischer (KF) reagent to a visually or
electrometrically determined endpoint that persists for
30 seconds. Add 98 mL (100 g) of sample, taking care
to protect the sample and contents of the flask from
moisture. Stir vigorously and titrate with Karl Fischer
reagent to the same endpoint.
% Water H
2
O
()
=
mL KF rea
g
ent
×
KF facto
r
g
H
2
OmL
()
×
100
Wei
g
ht of sam
p
le
g
()
8.4 Free Amines — Weigh 63 mL (65 g) of sample
into a 500 mL beaker. Add 100 mL of 2-propanol and
mix thoroughly. Into the solution, insert a pH and
reference electrodes connected to a pH meter set to the
direct voltage mode. Titrate potentiometrically with
0.05 N hydrochloric acid in 2-propanol. Express the
result in terms of methylamine:
% Free Amines as CH
3
N
H
2
()
=
mL
×
N
of HCl
×
3.10
Weight of sample g
(
)
8.5 Chloride — In a 50 mL glass-stoppered graduated
cylinder, dilute 24.5 mL (25 g) of sample with water to
volume. Place a 10 mL aliquot of this solution into a 50
mL Nessler tube and a 30 mL aliquot into a second
tube. To the first tube add 0.01 mg of chloride standard
and mix. Dilute the contents of each tube to about 45
mL with water, mix, add 1 mL of nitric acid and 1 mL
of silver nitrate reagent solution, mix thoroughly, and
allow to stand for 10 minutes. Any turbidity produced
by the sample should be no greater than that of the 0.01
mg standard.
8.6 Phosphate — Add 20 mL (20) of sample to 100
mL of dilute ammonium hydroxide (1 + 4). Prepare a
standard containing 0.1 mg of phosphate ion (PO
4
) in
100 mL of dilute ammonium hydroxide. Proceed as
follows with each of the two solutions.
8.6.1 Add, while stirring vigorously, 3.5 mL of a 10%
solution of ferric nitrate 9-hydrate. Allow to stand for
15 minutes. If the precipitate has not coagulated by this
time, warm gently (avoid boiling). Filter and wash the
precipitate on the filter with several portions of quite
dilute ammonium hydroxide (1 + 9). Discard the filtrate
and washings. Dissolve the precipitate on the filter with
50 mL nitric acid (1 + 3) added in small portions. Catch
the filtrate in a 250 mL glass-stoppered conical flask.
Add 13 mL of ammonium hydroxide (28-32% NH
3
) to
the flask while swirling and continue agitation until any
precipitate redissolves. Warm the solution to 40°C and
add 50 mL of ammonium molybdate-nitric acid reagent
solution. Shake vigorously for 5 minutes and allow to
stand at 40°C for 2 hours. The precipitate, if any, for
the sample should be no greater than that for the
standard.
8.6.2 Ammonium Molybdate-Nitric Acid Reagent
Solution — Mix thoroughly 100 g of molybdate acid,
85%, with 240 mL of water and 140 mL of ammonium
hydroxide (28 - 32% NH
3
). Filter and add 60 mL of
nitric acid. Cool and while stirring continually, pour
into a cooled mixture of 400 mL of nitric acid and 960
mL of water. Add 0.1 g of ammonium phosphate,
monobasic, NH
4
H
2
PO
4
, allow to stand 24 hours and
filter through glass wool.
8.7 Arsenic and Antimony (as As) — Evaporate 20 mL
(20 g) of sample in a 150 mL beaker to a small volume
on a hot plate. Cool, add carefully 15 mL of nitric acid
and 5 mL of sulfuric acid, and evaporate to dense fumes
of sulfur trioxide. Add 10 mL of nitric acid and again
evaporate to dense fumes. If carbon is still present,
cool, add 1 mL of 30% hydrogen peroxide, and
evaporate to dense fumes of sulfur trioxide. Repeat this
step with hydrogen peroxide addition until carbon has
been removed completely. Cool, and cautiously wash
the colorless residue 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 the sentence that
begins “Swirl the flask...”. Any red color in the silver
diethyldithiocarbamate solution of the sample should be
no greater than that of the standard containing 0.002 mg
of arsenic (As).
8.8 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), 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.
8.8.1 Special Reagents
8.8.1.1 Hydrochloric Acid, Ultra Pure — Use
hydrochloric acid specified for ultra low metal ion
content.
8.8.1.2 Mannitol Powder — Use mannitol specified
for reagent grade (A.C.S.) and determined, via the
reagent blank, to be ultra metal ion content.
8.8.1.3 5% Mannitol Solution — Dissolve and dilute 5
g of mannitol to 100 mL using water meeting the
criteria for Type E1.1 in ASTM D5127.
8.8.1.4 2% (v/v) Hydrochloric Acid Solution — Dilute
20 mL of ultra pure, 12 M hydrochloric acid to 1 L
using water meeting the criteria for Type E1.1 in
ASTM D5127.
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.