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SEMI C3.6-070 1 © SEMI 1981, 2001 2 4.1.4.4 C alculation of Conce ntrations 4.1.4.4.1 C arbon Monoxide an d Carbon D ioxide — Compare th e average peak areas for the calibration standard t o thos e of the phosphin e samp…

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SEMI C3.6-0701 © SEMI 1981, 20011
SEMI C3.6-0701
SPECIFICATION FOR PHOSPHINE (PH
3
) IN CYLINDERS, 99.98%
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 April 30, 2001. Initially available at www.semi.org May 2001; to be published July 2001.
Originally published in 1981; previously published in 1995.
1 Description
1.1 Phosphine is a highly toxic, flammable, colorless
gas with an odor of decaying fish. In high
concentrations, it is pyrophoric. It is shipped as a liquid
in cylinders under its own vapor pressure.
2 Specifications
QUALITY: 99.98%
Impurities
Maximum Acceptable
Level (ppm)*
Arsine (AsH
3
)10
Carbon dioxide (CO
2
)10
Carbon Monoxide (CO) 1
Heavy Metals **
Hydrogen (H
2
) 100
Nitrogen (N
2
)50
Oxygen (O
2
) + Argon (Ar) 5
Particles **
Hydrocarbons expressed as
Methane (C
1
–C
2
)
4
Water (H
2
O) (v/v) 1
TOTAL LISTED IMPURITIES 181
* 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.
** To be determined between supplier and user.
3 Physical Constants (for in formation only)
Metric Units US Units
Molecular weight 33.997 33.997
Boiling point at 1 atm -87.7°C -125.9°F
Density of gas at 25°C
(77°F) and 1 atm
1.402 kg/m
3
0.0875 lb/ft
3
Specific gravity of gas
at 21.1°C (70°F) and 1
atm (air = 1)
1.146 1.146
Density of liquid at
boiling point
744 kg/m
3
46.45 lb/ft
3
4 Analytical Procedures
4.1 Carbon Monoxide, Carbon Dioxide, and
Hydrocarbons (expressed as methane) — This
procedure is for the determination of carbon monoxide,
carbon dioxide, and hydrocarbons in phosphine 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 3.2
mm (1/8 in) OD by 2.2 mm (0.085 in) ID ss or
equivalent.
4.1.2.2 Carrier Flow — 35 mL/min helium.
4.1.2.3 Support Gases
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. *These
components are for reference only.
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.
4.1.4.2 Inject the sample to be tested in the same
manner as the calibration standard. Vent the phosphine
after the ethylene peak. Record the retention times and
peak areas.
4.1.4.3 Repeat 4.1.4.1.
SEMI C3.6-0701 © SEMI 1981, 2001 2
4.1.4.4 Calculation of Concentrations
4.1.4.4.1 Carbon Monoxide and Carbon Dioxide —
Compare the average peak areas for the calibration
standard to those of the phosphine sample being tested.
Calculate the concentration of each impurity, using the
formula below. The results may not exceed the
specification in Section 2 of this standard.
Sample
ofion Concentrat
Standard
ofion Concentrat
AreaPeak Standard
AreaPeak Sample
=×
4.1.4.4.2 Total Hydrocarbons Expressed as Methane
(C
1
–C
2
) — Compare the peak area of methane in the
calibration standard with the sum of the areas of the
hydrocarbons detected in the phosphine sample.
Calculate the concentration of total hydrocarbons using
the formula below. The results may not exceed the
specifications in Section 2 of this standard.
Sample of
ionConcentrat THC
Standardin
Methane ofion Concentrat
Methanefor
AreaPeak Standard
detected nsHydrocarbo
allfor areas of Sum
=×
4.2 Hydrogen, Nitrogen, and Oxygen + Argon, Arsine
— This procedure is for the determination of hydrogen,
nitrogen, oxygen + argon, and arsine in phosphine
using a gas chromatograph with a discharge ionization
detector. (See Note 2 and Figure 2.)
4.2.1 Detection Limits — 100 ppb (mol/mol)
hydrogen, 100 ppb (mol/mol) oxygen + argon, 500 ppb
(mol/mol) nitrogen, 5 ppm (mol/mol) arsine.
4.2.2 Instrument Parameters
4.2.2.1 Columns:
Column 1: Porapak QS, 2.5 m (8 ft) by 3.2 mm (1/8 in)
OD by 2.2 mm (0.085 in) ID ss or equivalent.
Column 2: Molecular Sieve 5A, 3 m (10 ft) by 3.2 mm
(1/8 in) OD by 2.2 mm (0.085 in) ID ss or
equivalent.
4.2.2.2 Carrier Flow — 25 mL/min helium.
4.2.2.3 Temperatures
Detector 10°C
Injector 30°C
Oven 40°C
4.2.2.4 Sample Volume — 1 mL.
4.2.3 Calibration Standard — 5–50 ppm (mol/mol)
nitrogen, 1–10 ppm (mol/mol) oxygen, 1–10 ppm
(mol/mol) argon, 10–100 ppm (mol/mol) hydrogen,
5–10 ppm (mol/mol) arsine, balance helium.
4.2.4 Operating Procedure
4.2.4.1 Determination of the Switching Time — Inject
the calibration sample in 4.2.3 above and note the time
when the hydrogen peak appears through detector B.
Switching valve 1 at that time will give an arsine peak
through detector A and hydrogen, oxygen + argon, and
nitrogen peaks through detector B.
4.2.4.2 Inject the calibration standard into the column
using the same gas valve. Switch at the time determined
in 4.2.4.1 and record retention times and peak areas.
Order of elution is hydrogen, oxygen + argon, and
nitrogen on detector B. Order of elution is phosphine
and arsine on detector A.
4.2.4.3 Inject the sample being tested in same manner
as the calibration standard. Record the retention times
and peak areas.
4.2.4.4 Repeat 4.2.4.2.
4.2.4.5 Compare the average peak areas of the
calibration standard to those of the phosphine 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 Peak Are
a
Standard Peak Area
×
Concentratio
n
of Standard
=
Concentratio
n
of Sample
4.3 Water — This procedure is for the determination
of moisture in phosphine using continuous flow
electrolysis of water in a phosphorous pentoxide (P
2
O
5
)
cell, modified as per the manufacturer’s
recommendation, for use with phosphine.
4.3.1 Detection Limit — 0.5 ppm (vol/vol).
4.3.2 Instrument Parameters
4.3.2.1 Flow Requirements — Set the sample flow rate
and pressure in accordance with manufacturer’s
instructions.
4.3.3 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 dew point/frost point
hygrometer. Standards are prepared in nitrogen.
4.3.4 Operating Procedure
4.3.4.1 Obtain representative sample of gas to analyze
and direct to unit as with the standards.
4.3.4.2 Determine the moisture content in sample gas
by comparing the indicated concentration with the
calibration curve constructed in 4.3.4.1. The result may
not exceed the specification in Section 2 of this
standard.
SEMI C3.6-0701 © SEMI 1981, 20013
4.4 Notes
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.
NOTE 2: Carrier gas purity of helium must be 99.9999%.
Figure 1
G.C. Configuration
Figure 2
Column Configuration for H
2
, N
2
, and O
2
+ Ar, AsH
3
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