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SEMI C60-0305 © SEMI 2005 6 9.5.2.2 Carrier Flow: 50 mL/min helium. 9.5.2.3 S ample Volume: 1.0 to 3.0 mL. 9.5.2.4 Temperatures: Detector 125°C Column Temperature 65°C 9.5.3 Calibration S tandards — 5–20 ppm (m ol/mol) n…

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9.3.4 Calibration Standards — 1–5 ppm (mol/mol) methane in helium, 1–5 ppm (mol/mol) ethane in helium, 1–5
ppm (mol/mol) ethylene, 1–5 ppm (mol/mol) propane, 1–5 ppm (mol/mol) acetylene, 1–5 ppm (mol/mol) propylene,
1–5 ppm (mol/mol) n-butane, and 1–5 ppm (mol/mol) n-pentane, balance in helium.
9.3.5 Operating Procedure
9.3.5.1 Inject the calibration standard into the column using a gas sampling valve. Record the retention time and
peak area.
9.3.5.2 Inject the sample to be tested in same manner as the calibration standard. Record the retention times and
peak areas.
9.3.5.3 Repeat ¶9.3.5.1.
9.3.5.4 Compare the average peak area of the calibration standard to that of the nitrous oxide sample being tested.
Calculate the concentration of hydrocarbons C
1
–C
5
, using the formula below. The result may not exceed the
specification in Table 1 of this Standard.
Sample Pea
k
Area
Standard Peak Area
Concentration
of Standard
Concentration
of Sample
9.4 Nitric Oxide — This procedure is for the determination of nitric oxide in nitrous oxide using
chemiluminescence. The detector shall have a photomultiplier tube capable of sensing the light emission of the
decaying nitrous oxide. The detector shall have variable attenuation, zero and span adjustments, display, and an
onboard ozone generator.
NOTE 3: This method does not determine nitrous oxide impurities.
9.4.1 Detection Limit — 0.1 ppm (mol/mol).
9.4.2 Instrument Parameters
9.4.2.1 Flow Requirements — Set the zero gas, span gas, and sample gas in accordance with the instrument
manufacturer’s instructions.
9.4.3 Calibration Standards
9.4.3.1 Zero argon (99.99% minimum) with less than 0.1 ppm nitric oxide.
9.4.3.2 The upper level argon span gas (99.99% minimum) not exceeding 5 times the concentration of the
specification.
9.4.3.3 The oxygen supplied to the ozone generator will contain less than 0.1 ppm nitric oxide.
9.4.4 Operating Procedure
9.4.4.1 Introduce the zero argon and set the instrument to zero with the zero adjust knob.
9.4.4.2 Introduce the span gas in argon and, using the span adjust knob, set the output reading to match the level of
nitric oxide in the span gas.
9.4.4.3 Repeat ¶9.4.4.1 and ¶9.4.4.2 until reproducibility of readings is better than 1% full scale.
9.4.4.4 Introduce the nitrous oxide sample into the analyzer and read the quantity of nitric oxide. The result may
not exceed the specification in table 1 of this standard.
9.5 Nitrogen and Oxygen — This procedure is for the determination of nitrogen and oxygen in nitrous oxide using a
gas chromatograph with a helium ionization detector.
9.5.1 Detection Limit — 0.5 ppm (mol/mol).
9.5.2 Instrument Parameters
9.5.2.1 Columns: Column 1: Porapak Q, 1.9 m (6 ft) by 3.2 mm (1/8 in) OD by 2.2 mm (0.085 in) ID stainless steel,
or equivalent. Column 2: Molecular sieve 5A, 2.4 m (8 ft) by 3.2 mm (1/8 in) OD by 2.2 mm (0.085 in) ID stainless
steel, or equivalent.
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9.5.2.2 Carrier Flow: 50 mL/min helium.
9.5.2.3 Sample Volume: 1.0 to 3.0 mL.
9.5.2.4 Temperatures:
Detector 125°C
Column Temperature 65°C
9.5.3 Calibration Standards — 5–20 ppm (mol/mol) nitrogen in helium and 1–5 ppm (mol/mol) oxygen in helium.
9.5.4 Operating Procedure
9.5.4.1 Inject the calibration standard into the column using a gas sampling valve. Record the retention time and
peak area.
9.5.4.2 Inject the sample to be tested in same manner as the calibration standard. Record the retention times and
peak areas.
9.5.4.3 Repeat ¶9.5.4.1.
9.5.4.4 Compare the average peak area of the calibration standard to that of the nitrous oxide sample being tested.
Calculate the concentrations of nitrogen and oxygen, using the formula below. The result may not exceed the
specification in Table 1 of this standard.
Sample Pea
k
Area
Standard Peak Area
Concentration
of Standard
Concentration
of Sample
9.6 Nitrogen Dioxide — This procedure is for the determination of nitrogen dioxide in nitrous oxide using an
apparatus employing a detector tube filled with a color-reactive chemical.
9.6.1 Detection Limit — 0.05 ppm.
9.6.2 Apparatus
9.6.2.1 Pressure Regulator: Outlet Pressure Range 0–30 psig.
9.6.2.2 Flowmeter: Range 0–200 mL/min.
9.6.2.3 Detector tube: Range 0.2–6 ppm.
9.6.2.4 Stop Watch.
9.6.2.5 6 mm (1/4 in) flexible tubing.
9.6.3 Operating Procedure
9.6.3.1 Attach a suitable regulator to the cylinder outlet.
9.6.3.2 Connect the flowmeter to the regulator using flexible tubing.
9.6.3.3 Open the cylinder valve and purge the flowmeter with nitrous oxide.
9.6.3.4 After the line is thoroughly purged, stop the flow of nitrous oxide and attach the detector tube to the outlet
of the flowmeter.
9.6.3.5 Start the flow of nitrous oxide and set the flow rate to 100 mL/min. The pressure and temperature of the
sample must be within the tolerance specified by the manufacturer.
9.6.3.6 Pass 800 mL of gas through the detector tube.
9.6.3.7 Determine the concentration of nitrogen dioxide according to the detector tube manufacturer's instructions.
The concentration may not exceed the specification in Table 1 of this standard.
9.7 Water — This procedure is for the determination of trace moisture (water) in nitrous oxide using a
piezoelectronic hygrometer.
SEMI C60-0305 © SEMI 2005 7
9.7.1 Detection Limit — 1.0 ppm (vol/vol).
9.7.2 Flow Requirements — Follow the flow requirements specified in the manufacturer’s instrument operation
manual.
9.7.3 Calibration Standards — 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.
NOTE 4: Other hygrometers may also be used, e.g. CRDS, FTIR, TDLAS, and vibrating quartz.
9.7.4 Sample System and Proper Operation
9.7.4.1 The sample system shall be as shown in Figure A1-2.
9.7.4.2 Attach sample system to nitrous oxide cylinder.
9.7.4.3 Partially open valve 2.
9.7.4.4 Open valve 1 and adjust pressure to 50 psig, ± 5 psig.
9.7.4.5 Adjust valve 2 until a flow of 500 mL/min, ± 50 mL/min is venting.
9.7.4.6 Tubing, valves and fittings are to be cleaned and passivated 316 stainless steel.
9.7.4.7 Keep tubing lengths to a minimum.
9.7.5 Operating Procedure
9.7.5.1 Follow the procedures outlined in the instrument manufacturer’s manual.
9.7.5.2 Allow the system to run until a stable reading is obtained for ten minutes.
9.7.5.3 Read the quantity of water on the analyzer meter. The result may not exceed the specification in Table 1 of
this standard.