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SEMI C59-1104 © SEMI 2002, 2004 5 12.1.2.4 Temperatures : Detector 280°C Column Oven 250°C 12.1.3 Calibration Stand ard — 1–5 ppm carbo n monoxide , 1–5 ppm hydr ogen in nitroge n. 12.1.4 Operating Procedure 12.1.4.1 Inj…

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piezoelectric moisture hygrometer until a stable reading
is obtained.
9.5.5 Determine the moisture content of the nitrogen
sample by comparing the reading to calibration curve.
The result may not exceed the specification in Table 1.
10 Analytical Procedures for Grade 5.2
Nitrogen (See Notes 1 and 2 in Section 9)
10.1 Carbon Monoxide and Carbon Dioxide — Use
the procedure in Section 9.1 for the analysis of carbon
monoxide and carbon dioxide.
10.1.1 Hydrogen — Use the procedure in Section 9.2
for the analysis of hydrogen.
10.1.2 Oxygen — Use the procedure in Section 9.3 for
the analysis of oxygen except that the standard should
be between 1 and 5 ppm oxygen in nitrogen.
10.1.3 Total Hydrocarbons — Use procedure Section
9.4 for the determination of total hydrocarbons except
that the calibration standard should be at the 0.1 ppm
level.
10.1.4 Water — This procedure is for the
determination of moisture (water) in nitrogen using a
continuous flowing, cooled-surface condensation,
dewpoint/ frostpoint hygrometer. (See NOTE 7 in
Section 9.)
NOTE 8: The National Institute of Standards and Technology
(NIST) provides calibration services for the thermometers
used in dewpoint/frostpoint hygrometers.
NOTE 9: This method is not applicable if other constituents
in the gas will condense before water vapor, e.g., carbon
dioxide and/or oil contamination.
10.1.4.1 Detection Limit — 0.6 ppm (vol/vol) or
79C (110F).
10.1.4.2 Flow Requirements
10.1.4.2.1 Set sample flow rate and pressure in
accordance with the instrument manufacturer's
instructions.
10.1.4.2.2 Gas must flow past the chilled mirror where
optic means are provided to detect the deposit (or frost)
and to read the thermometer measuring the temperature
of the mirror.
10.1.4.3 Calibration Standard — A calibration
thermometer designed to indicate temperatures in the
79C (110F) range required.
10.1.4.4 Operating Procedure
10.1.4.4.1 Obtain a continuous flow of sample gas
from the source using a clean stainless steel (or copper)
sampling line which has been purged dry after exposure
to ambient moisture.
10.1.4.4.2 After prepurging with a dry gas, allow the
sample gas to flow through the sampling system and the
dewpoint/frostpoint hygrometer for one hour to 24
hours to allow the entire system to reach equilibrium
with regard to moisture content.
10.1.4.4.3 After equilibrium has been reached, cool
down the mirror to determine the actual
dewpoint/frostpoint of the sample gas. Follow the
manufacturer’s recommendations to create the
temperatures needed.
10.1.4.4.4 Continue to verify the dewpoint/frostpoint
for at least 30 minutes after a stable reading has been
confirmed.
10.1.4.4.5 Correct the dewpoint reading from the
measured pressure to 1 atm of pressure. The result may
not exceed the specification in Table 1.
11 Analytical Procedures for Grade 5.4
Nitrogen (See Notes 1 and 2 in Section 9)
11.1 Carbon Monoxide and Carbon Dioxide — Use
the procedure in Section 9.1 for the analysis of carbon
monoxide and carbon dioxide.
11.2 Hydrogen — Use the procedure in Section 9.2 for
the analysis of hydrogen.
11.3 Oxygen — Use the procedure in Section 9.3 for
the analysis of oxygen except that the standard should
be between 0.5 and 2.5 ppm oxygen in nitrogen.
11.4 Total Hydrocarbons
— Use procedure Section 9.4
for the determination of total hydrocarbons except that
the calibration standard should be at the 0.1 ppm level.
11.5 Water — Use procedure in Section 9.5 for the
determination of water.
12 Analytical Procedures for Grade 5.5
Nitrogen (See Notes 1 and 2 in Section 9)
12.1 Carbon Monoxide and Hydrogen — This
procedure is for the determination of carbon monoxide
and hydrogen in nitrogen using a gas chromatograph
with a reduction gas detector (See Note 3 in Section
9.1).
12.1.1 Detection Limits — 2 ppb carbon monoxide, 20
ppb hydrogen.
12.1.2 Instrument Parameters
12.1.2.1 Column — 5A molecular sieve, 0.9 m (3 ft)
by 3 mm (1/4 in) stainless steel, or equivalent.
12.1.2.2 Carrier Flow — 40 mL/min air or nitrogen.
12.1.2.3 Sample Volume — 2.0 mL.
SEMI C59-1104 © SEMI 2002, 2004 5
12.1.2.4 Temperatures:
Detector 280°C
Column Oven 250°C
12.1.3 Calibration Standard — 1–5 ppm carbon
monoxide, 1–5 ppm hydrogen in nitrogen.
12.1.4 Operating Procedure
12.1.4.1 Inject the calibration standard into the column
using a gas sampling valve. Record the retention times
and peak areas. Order of elution is hydrogen, then
carbon monoxide. Run standard analysis in triplicate
for stability determination relative to purging of
calibration system components.
12.1.4.2 Inject the sample to be tested in same manner
as the calibration standard. Record the retention times
and peak areas.
12.1.4.3 Repeat Section 12.1.4.1.
12.1.4.4 Compare the average peak areas of the
calibration standard to that of the nitrogen sample being
tested. Calculate the concentrations of carbon
monoxide and hydrogen, using the formula:
Sample Peak Area
Concentration of Standard
Standard Peak Area
Concentration of Sample
12.1.4.5 The result may not exceed the specification in
Table 1.
12.2 Carbon Dioxide — This procedure is for the
determination of carbon dioxide in nitrogen using a
continuous flow, non-dispersive infrared analyzer.
12.2.1 Detection Limit — 50 ppb
12.2.2 Set sample flow rate and pressure in accordance
with the instrument manufacturer's instructions.
12.2.3 Calibration Standard — Zero nitrogen with a
known quantity of carbon dioxide at not more than 0.05
ppm. Span gas nitrogen with a known concentration of
1–10 ppm carbon dioxide.
12.2.4 Operating Procedure
12.2.4.1 Do not change the initial sample flow setting
once established.
12.2.4.2 Introduce the zero nitrogen with known
quantity of carbon dioxide and set the needle (or output
reading) to read the correct level using the zero
adjustment knob.
12.2.4.3 Introduce the span gas standard in nitrogen
and using the span adjust knob, set the needle (or output
reading) to match the levels of carbon dioxide in the
span gas.
12.2.4.4 Repeat Section 12.2.4.2 and Section 12.2.4.3
until reproducibility of readings is better than 1% of full
scale.
12.2.4.5 Introduce nitrogen sample into the analyzer
and read the quantity of carbon dioxide on the analyzer
meter. The result may not exceed the specification in
Table 1.
12.3 Oxygen — This procedure is for the determination
of oxygen in nitrogen using a continuous flow analyzer
using an electrochemical method.
12.3.1 Detection Limit — 50 ppb
12.3.2 Set sample pressure and flow rates in
accordance with the instrument manufacturer's
instructions.
12.3.3 Calibration Standard — 1–10 ppm oxygen in
nitrogen or accordance with the instrument
manufacturer's instructions.
12.3.4 Operating Procedure
12.3.4.1 Do not change the initial sample flow setting
once established.
12.3.4.2 Introduce nitrogen containing less than 2 ppm
oxygen through a deoxygenation catalyst to verify that
there is no leakage of air into the system and to
demonstrate that the detection limit can be achieved.
12.3.4.3 Introduce the calibration standard. Using the
span adjust knob, set the needle (or output reading) to
match the level of oxygen in the calibration gas.
12.3.4.4 Introduce nitrogen sample and record the
oxygen reading. The result may not exceed the
specification in Table 1.
12.4 Water — This procedure is for the determination
of trace moisture (water) in nitrogen using a continuous
flowing piezoelectric hygrometer (See NOTE 7 in
Section 9.5).
12.4.1 Detection Limit — 0.1 ppmv or 90°C
(130°F).
12.4.2 Flow Requirements — Set sample pressure and
flow rate in accordance with the instrument
manufacturer’s instructions.
12.4.3 Calibration Standard — Construct a calibration
curve which contains at least three points covering the
range of interest. The standards employed will be
verified independently by another analytical method.
12.4.4 Operating Procedure
12.4.4.1 Obtain a continuous flow of sample gas from
the source using a clean and passivated 316 stainless
steel line which has been purged dry after exposure to
ambient moisture.
SEMI C59-1104 © SEMI 2002, 2004 6
12.4.4.2 After prepurging with a dry gas, allow the
sample gas to flow through the sampling system and the
piezoelectric moisture hygrometer until a stable reading
is obtained. The result may not exceed the specification
in Table 1.
12.5 Total Hydrocarbons — This procedure is for the
determination of total hydrocarbons in nitrogen using a
continuous flow flame ionization detector-equipped
total hydrocarbon analyzer (See Notes 4, 5, and 6 in
Section 9.4).
12.5.1 Detection Limit — 0.1 ppm
12.5.2 Flow Requirements
12.5.3 High-purity, hydrocarbon-free (less than 1.0
ppm) hydrogen: 35–40 mL/min or 40% hydrogen in
either helium or nitrogen matrix at 75–80 mL/min.
12.5.4 Dry, hydrocarbon-free (less than 1.0 ppm) air:
350–400 mL/min.
12.5.5 Set sample flow rates in accordance with the
instrument manufacturer's instructions.
12.5.6 Calibration Standards
12.5.6.1 Zero nitrogen with known quantity of
hydrocarbons at 0.1 ppm level.
12.5.6.2 Span Gas — Nitrogen with known quantity
(1–10 ppm) hydrocarbons.
12.5.7 Operating Procedure
12.5.7.1 Do not change the initial flow settings for
hydrogen, air and sample once established.
12.5.7.2 Introduce the zero nitrogen with known
quantity of hydrocarbons and, using the 0–10 ppm
range, set the needle (or output) to read the correct level
using the zero adjust knob.
12.5.7.3 Introduce the span gas standard in nitrogen
and, using the span adjust knob, set the needle (or
output reading) to match the level of hydrocarbons in
the span gas.
12.5.7.4 Repeat Section 12.5.7.2 and Section 12.5.7.3
until reproducibility of readings is better than 1% of full
scale.
12.5.8 Introduce nitrogen sample into the analyzer and
read the quantity of hydrocarbons on the analyzer
meter. The result may not exceed the specification in
Table 1.
13 Analytical Procedures for Grade 5.6
Nitrogen (See Notes 1 and 2 in Section 9)
13.1 Carbon Monoxide and Hydrogen — Use the
procedure in Section 12.1 for the determination of
carbon monoxide and hydrogen.
13.2 Carbon Dioxide — Use procedure Section 12.2
for the determination of carbon dioxide.
13.3 Oxygen
— Use procedure Section 12.3 for the
analysis of oxygen.
13.4 Water — Use procedure Section 9.5 for the
determination of water.
13.5 Total Hydrocarbons — Use procedure Section 9.4
for the determination of hydrocarbons, except that the
calibration standard should be at 0.1 ppm hydrocarbons.
14 Analytical Procedures for Grade 6.0
Nitrogen (See Notes 1 and 2 in Section 9)
14.1 Carbon Monoxide and Hydrogen — This
procedure is for the determination of carbon monoxide
and carbon dioxide in nitrogen using a gas
chromatograph fitted with a reduction gas detector.
(See NOTE 3 in Section 9.1.)
14.1.1 Detection Limit — Hydrogen 3 ppb, CO, 0.3
ppb
14.1.2 Instrument Parameters
14.1.2.1 Column 1 — 1/8” OD 77” length Unibead 1S
60–80 mesh, Column 2 — 1/8” OD 30 ¾” length
MS5A
14.1.2.2 Carrier Flow — 20 mL/min at 105°C
nitrogen.
14.1.2.3 Sample Volume — 100 µL
14.1.2.4 Temperatures:
Detector 270°C
Column Oven 105°C
14.1.3 Calibration Standards — 0.1–0.5 ppm carbon
monoxide, 0.1–0.5 ppm hydrogen, balance nitrogen.
14.1.3.1 Construct a calibration curve in the range of
interest. Verify the standards employed independently
by established traceability to recognized national or
international standards.
14.1.4 Operating Procedure
14.1.4.1 Inject the calibration standard into the column
using a gas sampling valve. Record the retention times
and peak areas. Order of elution is hydrogen, carbon
monoxide.
14.1.4.2 Inject the sample to be tested in same manner
as the calibration standard. Record the retention times
and peak areas.
14.1.4.3 Repeat Section 14.1.4.1.
14.1.4.4 Compare the average peak area of the
calibration standard to that of the nitrogen sample being