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SEMI C3.32-03 01 © SEMI 1987 , 2001 1 SEMI C3.32-0301 SPECIFICA TION FOR CHLORINE (Cl 2 ), 99.996% QUALITY This specif ication was technic ally approved by the Global Ga ses Committee and is the direct responsib ility of…

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SEMI C3.40-1000 © SEMI 1989, 2000 6
Figure 2
Configuration for the Analysis of SF
6
in CF
4
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SEMI C3.32-0301 © SEMI 1987, 20011
SEMI C3.32-0301
SPECIFICATION FOR CHLORINE (Cl
2
), 99.996% 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 1987; previously published in 1995.
1 Description
1.1 Gaseous chlorine is greenish-yellow and about 2.5
times as heavy as air. Chlorine has a disagreeable and
suffocating odor.
2 Specifications
QUALITY: 99.996%
Impurities
Maximum Acceptable Level
(ppm) (See NOTE 1.)
Carbon dioxide (CO
2
)10
Carbon monoxide (CO) 1
Hydrocarbons (C
1
– C
2
)1
Nitrogen (N
2
)20
Oxygen (O
2
)4
Water (H
2
O) (v/v) (See NOTE 2.)
TOTAL LISTED IMPURITIES
(excluding chromium, iron,
nickel, and sodium)
36
Maximum Acceptable Level
(ppm) (See NOTE 1.)
Chromium (Cr) 0.2 by wt. Liquid Phase
Iron (Fe) 0.2 by wt. Liquid Phase
Nickel 0.2 by wt. Liquid Phase
Sodium 1 by wt. Liquid Phase
NOTE 1: An analysis of significant figures has not been considered.
The number of significant figures will be based on analytical
accuracy and on the precision of the provided procedure.
NOTE 2: It is not known whether H
2
O remains as H
2
O in Cl
2
or
reacts to other species. For this reason, interpretation of H
2
O
measurement data is questionable. Test and acceptance criteria shall
be determined between user and supplier. Possible methods include:
a) determination of HCl by Fourier transform infrared spectrometry
(FTIR), mass spectrometry, or gas chromatography; b) measurement
of water by electrolysis in a P
2
O
5
cell (reported in terms of H
2
O
equivalents); c) determination of water by FTIR.
3 Physical Constants (for in formation only)
Metric Units US Units
Molecular weight 70.9 70.9
Boiling point at 1 atm -34.05°C -29.3°F
Density gas at 20°C (68°F)
and 1 atm
2.980 kg/m
3
0.1860 lb/ft
3
Specific gravity 2.473 2.473
Density liquid at -118°C
(-180.8°F)
1574.8 kg/m
3
98.26 lb/ft
3
4 Analytical Procedures
4.1 Carbon Monoxide, Carbon Dioxide, and
Hydrocarbons (CH
4
, C
2
H
2
, C
2
H
4
, C
2
H
6
) — This
procedure is for the determination of carbon monoxide,
carbon dioxide, and C
1
–C
2
hydrocarbons in chlorine.
The sample shall be vapor phase and analyzed using a
gas chromatograph with a flame ionization detector/
methanizer combination. (See Figure 1 and Notes 1, 2,
and 3.)
4.1.1 Detection Limit — 0.1 ppm (mol/mol).
4.1.2 Instrument Parameters
4.1.2.1 Injection Valve — 10 port corrosion-resistant.
4.1.2.2 Sample Volume — 2 mL.
4.1.2.3 Columns:
Column 1: Porapak P, 3.1 m (10 ft) by 3.2 mm (1/8 in) OD
ss or equivalent.
Column 2: Porapak P, 3.1 m by 3.2 mm OD ss or
equivalent.
4.1.2.4 Carrier Flow — 20 mL/min nitrogen.
4.1.2.5 Column Temperature — 40°C.
4.1.2.6 Air and Hydrogen Pressure and Flow — As
specified by the instrument manufacturer.
4.1.3 Calibration Standard — 1–5 ppm (mol/mol)
each component in nitrogen.
4.1.4 Operating Procedure
4.1.4.1 Place the 10 port valve in the sample load
position.
4.1.4.2 Turn on the methanizer heater and establish
hydrogen flow. Allow unit to heat to operating
temperature (as specified by the manufacturer).
4.1.4.3 Establish air flow and ignite burner following
the instrument manufacturer’s instructions. Allow the
system to stabilize for 15 minutes.
SEMI C3.32-0301 © SEMI 1987, 2001 2
4.1.4.4 Determine the time at which ethane elutes
from the first column and absorbs onto the second
column so one can vent the chlorine. Inject the
calibration ethane standard and record the retention
time of ethane obtained without returning the valve to
the load position. Multiply this time by 0.6. The result
will be the time during the analysis at which the
injection valve should be returned to the load position,
backflushing the chlorine to vent.
Repeat the injection of the ethane calibration standard,
including the backflush, to ensure that enough time has
passed to allow elution of ethane onto the second
column.
4.1.4.5 Inject the remaining standards using the
backflush technique. Record the retention times and
peak areas.
4.1.4.6 Analyze the chlorine sample to be tested in the
same manner as in 4.1.4.5. Repeat the sample injection
until peak areas of the impurity of interest agree within
5%.
4.1.4.7 Analyze each of the calibration standards again
as in 4.1.4.5.
4.1.4.8 Compare the average peak areas of the
calibration standards to those of the chlorine 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 Are
a
×
Concentratio
n
of Standard
=
Concentratio
n
of Sample
4.2 Oxygen and Nitrogen — This procedure is for the
determination of oxygen and nitrogen in chlorine. The
sample shall be vapor phase and analyzed using a gas
chromatograph with a thermal conductivity detector.
(See Figure 2 and Notes 1 and 2.)
4.2.1
Detection Limits — 2 ppm (v/v) oxygen, 5 ppm
(v/v) nitrogen.
4.2.2
Instrument Parameters
4.2.2.1 Injection Valve — 10 port corrosion-resistant.
4.2.2.2
Sample Volume — 2 mL.
4.2.2.3 Columns:
Column 1: Porapak Q, 1.8 m (6 ft) by 3.2 mm (1/8 in)
OD ss or equivalent.
Column 2: Molecular sieve 13×, 3.1 m (10ft) by 3.2 mm
OD ss or equivalent.
4.2.2.4 Carrier Flow — 20 mL/min he lium.
4.2.2.5
Temperature:
Column 30°C
Detector 50°C
4.2.3 Calibration Standard — 10–40 ppm (v/v) each
component in helium.
4.2.4
Operating Procedure
4.2.4.1 Place the 10 port valve in the sample load
position.
4.2.4.2 Inject the standard, wait one minute, then
return the valve to the sample load position to backflush
the principal gas to vent while allowing the oxygen and
nitrogen to pass to the analytical column. Record the
retention times and peak areas.
4.2.4.3
Inject the standard at least three times. All
peak areas for a specific impurity should agree within
5%.
4.2.4.4
Inject the chlorine sample to be tested in the
same manner as in 4.2.4.2 and 4.2.4.3. Record the
retention times and peak areas.
4.2.4.5
Repeat 4.2.4.2 and 4.2.4.3.
4.2.4.6 Compare the average peak areas of calibration
standards with that of the chlorine sample being tested.
Calculate the concentrations of oxygen and nitrogen,
using the formula below. The results may not exceed
the specifications in Section 2 of this standard.
Sample Peak Are
a
Standard Peak Are
a
×
Concentratio
n
of Standard
=
Concentratio
n
of Sample
4.3
Trace Elements — This procedure gives
instructions for the determination of trace elements in
liquid phase chlorine using inductively coupled plasma
mass spectrometry (ICP-MS). (See Note 4.)
4.3.1
Detection Limit — (See Note 4.)
4.3.2 Instrument Parameters — (See Note 4.)
4.3.3 Calibration Standards — (See Note 4.) All
instrument calibration standards should be prepared
from NIST-traceable reference standards.
4.3.4
Sample Collection Apparatus — (See Notes 5
and 6 and Figures 3 and 4.)
4.3.4.1 Cylinder Connector — Stainless steel, or other
suitable material, dependent on the cylinder valve used.
4.3.4.2
Fluorocarbon Tubing — 6.4 mm (1/4") and 3.2
mm (1/8") outer diameters required, lengths dependent
on construction of apparatus.