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SEMI C3.2-030 1 © SEMI 1981, 2001 2 4.1.4.4 Co m pare the average peak are a s o f the calibration standard to those of the arsine sample being tested. C alculate the concentration of each i mpurity, using th e formula b…
SEMI C3.2-0301 © SEMI 1981, 20011
SEMI C3.2-0301
SPECIFICATION FOR ARSINE (AsH
3
) IN CYLINDERS, 99.94% QUALITY
This specification was technically approved by the Global Gases Committee and is the direct responsibility of
the North American Gases Committee. Current edition approved by the North American Regional Standards
Committee on October 17, 2000. Initially available at www.semi.org January 2001; to be published March
2001. Originally published in 1981; previously published in 1992.
1 Description
1.1 Arsine is a highly toxic, flammable, colorless gas
with a disagreeable garlic-like odor. It is a hemolytic
poison.
2 Specifications
QUALITY: 99.94%
Impurities
Maximum Acceptable
Level (ppm)
(See NOTE 1.)
Carbon monoxide and carbon dioxide
(CO + CO
2
)
2
Hydrocarbons (methane (CH
4
),
ethane (C
2
H
6
), ethylene (C
2
H
4
), and
acetylene (C
2
H
2
))
1
Hydrogen (H
2
) 500
Hydrogen Sulfide (H
2
S) 1
Nitrogen (N
2
)10
Oxygen (O
2
) + Argon (Ar) 5
Phosphine (PH
3
)10
Water (H
2
O) 4
TOTAL LISTED IMPURITIES 533
Metals — See NOTE 2.
Particles — See NOTE 2.
NOTE 1: An analysis of significant figures has not been considered.
The number of significant figures will be based on analytical
accuracy and the precision of the provided procedure.
NOTE 2: To be determined between supplier and user.
3 Physical Constants (for in formation only)
Metric Units US Units
Molecular weight 77.946 77.946
Boiling point at 1 atm -62.48°C -80.46°F
Density of gas at 20°C
(68°F) and 1 atm
3.243 kg/m
3
0.202 lb/ft
3
Specific gravity of gas at
21.1°C (70°F) and 1 atm
(air = 1)
2.695 2.695
Density of liquid at B.P. 1653 kg/m
3
103.96 lb/ft
3
4 Analytical Procedures
4.1 Carbon Monoxide, Carbon Dioxide, and
Hydrocarbons (methane, ethane, ethylene, acetylene)
— This procedure is for the determination of carbon
monoxide, carbon dioxide, and hydrocarbons in arsine
using a gas chromatograph with a methanizer and a
flame ionization detector. (See Note 1 and Figure 1.)
4.1.1 Detection Limit — 0.1 ppm each impurity.
4.1.2 Instrument Parameters
4.1.2.1 Column: Porapak QS, 3.5 m (12 ft) by 2 mm
ID (1/8 in OD) ss or equivalent.
4.1.2.2 Carrier Flow: 35 mL/min helium.
4.1.2.3 Support Gases: Set the flow rates as specified
by the instrument manufacturer.
Hydrogen: 30 mL/min added to the carrier gas
between the column outlet and the
methanizer inlet.
Air: 500 mL/min.
4.1.2.4 Temperatures:
Detector 110°C
Injector 40°C
Oven 40°C
Methanizer 370–400°C
4.1.2.5 Sample Volume: 3 mL.
4.1.3 Calibration Standards — 1–10 ppm each:
carbon monoxide, carbon dioxide, methane, ethane,
ethylene, and acetylene; balance helium.
4.1.4 Operating Procedure
4.1.4.1 Inject the calibration standard into the column
using a gas sampling valve. Record retention times and
peak areas. Order of elution is carbon monoxide,
methane, carbon dioxide, acetylene, ethylene, ethane.
4.1.4.2 Inject the sample to be tested in same manner
as the calibration standard. Vent the arsine after the
ethane peak. Record the retention times and peak areas.
4.1.4.3 Repeat 4.1.4.1.
SEMI C3.2-0301 © SEMI 1981, 2001 2
4.1.4.4 Compare the average peak areas of the
calibration standard to those of the arsine sample being
tested. Calculate the concentration of each impurity,
using the formula below. The results may not exceed
specifications in Section 2 of this Standard.
Sample Pea
k
Area
Standard Peak
Area
×
Concentration
of Standard
=
Concentration
of Sample
4.2 Phosphine — This procedure is for the
determination of phosphine in arsine using a gas
chromatograph with a thermal conductivity detector.
4.2.1 Detection Limit — 5 ppm (mol/mol).
4.2.2 Instrument Parameters
4.2.2.1 Column: Porapak QS, 3.5 m (12 ft) by 2 mm
ID (1/8 in OD) ss or equivalent.
4.2.2.2 Carrier Flow: 35 mL/min helium.
4.2.2.3 Temperatures:
Detector 80°C
Injector 40°C
Oven 40°C
4.2.2.4 Sample Volume: 3 mL.
4.2.3 Calibration Standard — 10–50 ppm (mol/mol)
phosphine, balance helium.
4.2.4 Operating Procedure
4.2.4.1 Inject the calibration standard into the column
using a gas sampling valve. Record the retention time
and peak area.
4.2.4.2 Inject the sample being tested in same manner
as the calibration standard. Record the retention time
and peak area.
4.2.4.3 Repeat 4.2.4.1.
4.2.4.4 Compare the average peak area of the
calibration standard to that of the arsine sample being
tested. Calculate the concentration of phosphine, using
the formula below. The result may not exceed the
specification in Section 2 of this Standard.
Sample Pea
k
Area
Standard Peak
Area
×
Concentration
of Standard
=
Concentration
of Sample
4.3 Hydrogen, Nitrogen and Oxygen + Argon — This
procedure is for the determination of hydrogen,
nitrogen, oxygen + argon in arsine using a gas
chromatograph with a helium ionization detector.
4.3.1 Detection Limits — 100 ppb (mol/mol)
hydrogen, 100 ppb oxygen + argon, 500 ppb nitrogen.
4.3.2 Instrument Parameters
4.3.2.1 Columns:
Column 1: Porapak QS, 2.5 m (8 ft) by 3.2 mm
(1/8 in) ID ss or equivalent
Column 2: Molecular Sieve 5A, 3 m (10 ft) by
3.2 mm ID ss or equivalent.
4.3.2.2 Carrier Flow: 25 mL/min helium.
4.3.2.3 Temperatures:
Detector 10°C
Injector 30°C
Oven 30°C
4.3.2.4 Sample Volume: 3 mL.
4.3.3 Calibration Standard — 1–10 ppm nitrogen, 1–
10 ppm oxygen, 1–10 ppm argon, 10–100 ppm
hydrogen, balance helium.
4.3.4 Operating Procedure
4.3.4.1 Determination of the backflush time: Inject a
methane sample (1–1000 ppm, balance helium) using a
10 port gas valve and backflush at different times.
Select the backflush time so that the methane peak is
split by the backflush.
4.3.4.2 Inject the calibration standard into the column
using the same gas valve. Backflush at the time
determined in 4.3.4.1 and record retention times and
peak areas. Order of elution is hydrogen, oxygen +
argon and nitrogen.
4.3.4.3 Inject the sample being tested in same manner
as the calibration standard. Record the retention times
and peak areas.
4.3.4.4 Repeat 4.3.4.2.
4.3.4.5 Compare the average peak areas of the
calibration standard to those of the arsine sample being
tested. Calculate the concentration of each impurity,
using the formula below. The results may not exceed
the specifications in Section 2 of this Standard.
Sample Pea
k
Area
Standard Peak
Area
×
Concentration
of Standard
=
Concentration
of Sample
4.4 Hydrogen Sulfide — This procedure is for the
determination of hydrogen sulfide in arsine using gas a
chromatograph with a flame photometric detector.
4.4.1 Detection Limit — 0.1 ppm (mol/mol).
SEMI C3.2-0301 © SEMI 1981, 20013
4.4.2 Instrument Parameters
4.4.2.1 Column: Porapak QS 3.5 m (12 ft) by 2 mm ID
(1/8 in OD) ss or equivalent.
4.4.2.2 Carrier Flow: 35 mL/min helium. Set the flow
rates as specified by the instrument manufacturer.
4.4.2.3 Support Gases:
Hydrogen: 30 – 40 mL/min.
Air: 300 – 400 mL/min.
4.4.2.4 Temperatures:
Detector 75°C
Injector 40°C
Oven 40°C
4.4.2.5 Sample Volume: 1.5 mL.
4.4.3 Calibration Standard — 1–10 ppm hydrogen
sulfide, balance helium.
4.4.4 Operating Procedure
4.4.4.1 Inject the calibration standard into the column
using a gas sampling valve. Record retention time and
peak area.
4.4.4.2
Inject the sample being tested in the same
manner as the calibration standard. Vent before arsine
peak is eluted using same configuration as in Figure 1.
4.4.4.3 Repeat 4.4.4.1
4.4.4.4 Compare the average peak area of the
calibration standard to those of the arsine sample being
tested. Calculate the concentration of the hydrogen
sulfide, using the formula below. The result may not
exceed the specification in Section 2 of this Standard.
Sample Pea
k
Area
Standard Peak
Area
×
Concentration
of Standard
=
Concentration
of Sample
4.5 Water — This procedure is for the determination
of moisture in arsine using continuous flow electrolysis
of water in a phosphorus pentoxide (P
2
O
5
) cell.
4.5.1 Detection Limit — 1 ppm (vol/vol).
4.5.2 Instrument Parameters
4.5.2.1 Flow Requirements — Set the sample flow rate
and pressure in accordance with manufacturer’s
instructions.
4.5.3
Calibration Standards — Construct a calibration
curve which contains at least three points covering the
range of interest. Verify the standards employed
independently on a condensation dewpoint/frostpoint
hygrometer.
4.5.4
Operating Procedure
4.5.4.1 Obtain representative sample of gas to be
analyzed and direct to unit as with the standards.
4.5.4.2 Determine the moisture content in the sample
gas by comparing the indicated concentration with the
calibration curve constructed in 4.5.3. The result may
not exceed the specification in Section 2 of this
Standard.
NOTE 1: Carrier gases should contain less than 0.1 ppm
(mol/mol) carbon monoxide and less than 0.1 ppm (mol/mol)
carbon dioxide.
Figure 1
G. C. Configuration
NOTICE:
This specification does not purport to
address safety issues, if any, associated with its use. It
is the responsibility of the user of this specification to
establish appropriate safety and health practices and
determine the applicability of regulatory limitations
prior to use. SEMI makes no warranties or
representations as to the suitability of the specification
set forth herein for any particular application. The
determination of the suitability of the specification is
solely the responsibility of the user. Users are cautioned
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product data sheets, and other relevant literature
respecting any materials or equipment mentioned
herein. This specification are subject to change without
notice.
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compliance with this specification may require use of
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