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SEMI C59-1104 © SEMI 2002, 2004 7 tested. Calculate the concentrations of carbon monoxide and hydro g en usi ng the form ula: Sam ple Peak Area Co nce ntratio n of Standard St andard Peak Area Concentrat ion of Samp le …

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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
SEMI C59-1104 © SEMI 2002, 2004 7
tested. Calculate the concentrations of carbon
monoxide and hydrogen using the formula:
Sample Peak Area
Concentration of Standard
Standard Peak Area
Concentration of Sample
14.1.4.5 The result may not exceed the specification in
Table 1.
14.2 Carbon Dioxide — This procedure is for the
determination of carbon dioxide in nitrogen using a gas
chromatograph with a flame ionization detector, fitted
with a methanizer.
14.2.1 Detection Limit — 2 ppb
14.2.2 Instrument Parameters
14.2.2.1 Column — 1/8” OD 77” Length Hayesep D
100-120 mesh.
14.2.2.2 Flow Rates:
Carrier Flow: 30 mL/min nitrogen
Air Flow: 250 mL/min
Hydrogen Flow: 30 mL/min
14.2.2.3 Sample Volume — 5 mL
14.2.2.4 Temperatures:
Methanizer 315°C
Column Temperature 40°C
14.2.3 Calibration Standard — 0.1 ppm carbon dioxide
in nitrogen.
14.2.3.1 Construct a calibration curve in the range of
interest. Verify the standards employed independently
by established traceability to recognized national or
international standards.
14.2.4 Operating Procedure
14.2.4.1 Inject the calibration standard into the column
using a gas sampling valve. Record the retention time
and peak area.
14.2.4.2 Inject the sample to be tested in same manner
as the calibration standard. Record the retention time
and peak area.
14.2.4.3 Repeat Section 14.2.4.1.
14.2.4.4 Compare the average peak area of the
calibration standard to that of the nitrogen sample being
tested. Calculate the concentration of carbon dioxide,
using the formula:
Sample Peak Area
Concentration of Standard
Standard Peak Area
Concentration of Sample
14.2.4.5 The result may not exceed the specification in
Table 1.
14.3 Oxygen — This procedure is for the determination
of oxygen in nitrogen using a continuous flow analyzer
using an electrochemical method.
14.3.1 Detection Limit — 2 ppb
14.3.2 Flow Rate — Set sample flow rates in
accordance with the instrument manufacturer's
instructions.
14.3.3 Calibration Standards — 50 ppb oxygen in
nitrogen or in accordance with the instrument
manufacturer’s instructions.
14.3.4 Operating Procedure
14.3.4.1 Introduce nitrogen sample and record oxygen
reading. The result may not exceed the specification in
Table 1.
14.4 Total Hydrocarbons — This procedure is for the
determination of total hydrocarbons in nitrogen using a
gas chromatograph fitted with a flame ionization
detector and a back flush valve.
14.4.1 Detection Limit — 2 ppb
14.4.2 Instrument Parameters
14.4.2.1 Column — 1/8” OD 77” Length Hayesep D
100-120 mesh.
14.4.2.2 Flow Rates:
Carrier Flow: 30 mL/min nitrogen
Air Flow: 250 mL/min
Hydrogen Flow: 30 mL/min
14.4.2.3 Sample Volume — 5 mL
14.4.2.4 Temperatures — Column Temperature 40°C
14.4.3 Calibration Standard — 0.1 ppm methane in
nitrogen.
14.4.3.1 Calibration Standards — Construct a
calibration curve in the range of interest. Verify the
standards employed independently by established
traceability to recognized national or international
standards.
14.5 Water — This procedure is for the determination
of trace moisture (water) in nitrogen using a continuous
flowing phosphorous pentoxide hygrometer. (See Note
7 in Section 9.5.)
14.5.1 Detection Limit — 10 ppbv
14.5.2 Flow Requirements — Set the sample pressure
and flow rate in accordance with the instrument
manufacturer’s instructions.
SEMI C59-1104 © SEMI 2002, 2004 8
14.5.3 Calibration Standards — Construct a calibration
curve in the range of interest. Verify the standards
employed independently by established traceability to
recognized national or international standards.
14.5.4 Operating Procedure
14.5.4.1 Obtain a continuous flow sample of gas from
the source using a clean and passivated stainless steel
line which has been purged dry after exposure to
ambient moisture.
14.5.4.2 After prepurging with a dry gas, allow the
sample gas to flow through the sampling system and the
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moisture hygrometer until a stable reading is
obtained.
14.5.4.3 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.
NOTICE: SEMI makes no warranties or
representations as to the suitability of the standards set
forth herein for any particular application. The
determination of the suitability of the standard is solely
the responsibility of the user. Users are cautioned to
refer to manufacturer’s instructions, product labels,
product data sheets, and other relevant literature
respecting any materials mentioned herein. These
standards are subject to change without notice.
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compliance with this standard may require use of
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