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SEMI C3.35-11 01 © SEMI 1988 , 2001 2 4.1.4.3 Inj ect the sam ple to be tested in same manner as the calib ration standard. Record the retention times and peak areas. Backflush the main com ponent at the time det ermined…

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SEMI C3.35-1101 © SEMI 1988, 20011
SEMI C3.35-1101
SPECIFICATION FOR HYDROGEN CHLORIDE (HCl), 99.997%
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 August 27, 2001. Initially available at www.semi.org September 2001; to be published
November 2001. Originally published in 1988; previously published in 1995.
1 Description
1.1 Hydrogen chloride is a colorless, pungent,
corrosive gas having a suffocating odor. Hydrogen
chloride is heavier than air and fumes strongly in moist
air. It is very soluble in water and alcohol, and also
soluble in ether. While in the cylinder under pressure,
hydrogen chloride is in the form of a gas over liquid. As
long as liquid is present in the cylinder, the pressure
will remain fairly constant. When the liquid phase is
exhausted, the cylinder pressure will drop rather
rapidly.
2 Specifications
QUALITY: 99.997% (See Notes 1, 2, and 3.)
Impurities
Maximum Acceptable
Level (ppm)*
Carbon dioxide (CO
2
)10
Hydrogen (H
2
)5
Nitrogen (N
2
)10
Oxygen (O
2
) + Argon (Ar) 1
Methane and Acetylene 1
Water (H
2
O) (v/v) 1
TOTAL LISTED IMPURITIES
(excluding metals)
28
Maximum Acceptable
Level (ppm)*
Iron (Fe) 1 wt. vapor phase
* 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 procedure provided.
NOTE 1: Due to the reactive nature of the material and the
impurities, this product should be used within a period which
may be specified by the supplier.
NOTE 2: It is recommended that the user discontinue the use
of a cylinder prior to complete consumption of the liquid
phase. The content of cylinders should be determined by
weight, not pressure.
NOTE 3: This specification applies to the gas phase of the
cylinder as received.
3 Physical Constants (for information only)
Metric Units US Units
Molecular weight 36.465 36.465
Boiling point at 1 atm –85.°C –121.°F
Density of gas at 21.1°C
(70°F) and 1 atm
1.522 kg/m
3
0.095 lb/ft
3
Specific gravity of gas at
0°C (32°F) and 1 atm
1.268 1.268
4 Analytical Procedures
4.1 Carbon Dioxide — This procedure is for the
determination of carbon dioxide in hydrogen chloride
using a gas chromatograph with a thermal conductivity
detector. A backflush is used to keep the main
component from reaching the detector.
4.1.1 Detection Limit — 2 ppm.
4.1.2 Instrument Parameters
4.1.2.1 Column: Porapak Q, 2.4 m (8 ft) by 6.4 mm
(1/4 in) OD ss or equivalent.
4.1.2.2 Carrier Flow: 40 mL/min helium.
4.1.2.3 Temperatures:
Detector 50°C
Column Oven 40°C
4.1.2.4 Sample Volume: 10 mL.
4.1.3 Calibration Standard — 100 ppm carbon dioxide
in helium.
4.1.4 Operating Procedure
4.1.4.1 To determine the backflush time, inject the
calibration standard, using a gas sampling valve.
Record the retention time for carbon dioxide. Choose
the backflush time so that the complete carbon dioxide
peak is eluted.
4.1.4.2 Inject the calibration standard into the column
using a gas sampling valve. Record the retention times
and peak areas. Backflush at the time determined in
Section 4.1.4.1.
SEMI C3.35-1101 © SEMI 1988, 2001 2
4.1.4.3 Inject the sample to be tested in same manner
as the calibration standard. Record the retention times
and peak areas. Backflush the main component at the
time determined in Section 4.1.4.1.
4.1.4.4 Repeat Section 4.1.4.2.
4.1.4.5 Compare the average peak area of the
calibration standard to that of the hydrogen chloride
sample being tested. Calculate the concentration of
carbon dioxide, using the formula below. The result
may not exceed the specification in Section 2 of this
Standard.
Sample Peak Area
Standard Peak Area
×
Concentration
of Standard
=
Concentratio
n
of Sample
4.2 Hydrogen — This procedure is for the
determination of hydrogen in hydrogen chloride using a
gas chromatograph with a thermal conductivity
detector.
4.2.1 Detection Limit — 3 ppm.
4.2.2 Instrument Parameters
4.2.2.1 Columns:
Column 1: Ascarite, 0.3 m (1 ft) by 9.6 mm (3/8 in)
OD ss or equivalent.
Column 2: Molecular Sieve 5A, 2.4 m (8 ft) by 6.4
mm (1/4 in) OD ss or equivalent.
4.2.2.2 Carrier Flow: 40 mL/min nitrogen.
4.2.2.3 Temperatures:
Detector 50°C
Column Oven 40°C
4.2.2.4 Sample Volume: 10 mL.
4.2.3 Calibration Standard — 50 ppm hydrogen in
nitrogen.
4.2.4 Operating Procedure
4.2.4.1 Inject the calibration standard using a gas
sampling valve. Record the retention time and peak
area.
4.2.4.2 Inject the sample to be 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 with that of the hydrogen chloride
sample being tested. Calculate the concentration of
hydrogen using the formula below. The result may not
exceed the specification in Section 2 of this standard.
Sample Peak Area
Standard Peak Area
×
Concentration
of Standard
=
Concentratio
n
of Sample
4.3 Iron — This procedure is for the determination of
iron sampled from gaseous hydrogen chloride and
analyzed by inductively coupled plasma.
4.3.1 Sampling Apparatus
• 3 Teflon diaphragm valves (1/4" FNPT)
(Fluoroware 201-10 or equivalent).
• 2 Teflon tees (1/4") (Fluoroware UT4FN-1 or
equivalent).
• 50 ft. Teflon tubing (1/4") (Fluoroware AT250-047
or equivalent).
• Teflon flow meter (1/4" FNPT calibrated for HCl
flow) (Fluoroware FM-4N-1P or equivalent).
• 8 Teflon connectors (1/4" tube to 1/4" MNPT
(Fluoroware C4-CFN-1 or equivalent).
• 9 gas washing bottles (375 mL) (Savillex #507 or
equivalent with 501-4-2 cap).
• Tee purge assembly (Matheson 4756-330 or
equivalent).
• Manual control valve (Matheson 55A-330 or
equivalent).
• Cylinder scale that can measure the mass of the
cylinder to ± 1 g accuracy.
4.3.2 Water — 18 megohm-cm DI water is used for all
dilution blanks and washings.
4.3.3 Reagents — All reagents are of the highest purity
available minimizing background metal contamination.
4.3.4 Sampling Gaseous Hydrogen Chloride
4.3.4.1 Assemble entire sampling apparatus (see Figure
1) in laboratory hood for safety.
4.3.4.2 Fill gas washing bottles (scrubbers) with 75 mL
18 mega-ohm DI water.
4.3.4.3 Start nitrogen purge to remove air from system
and to check for leaks.
4.3.4.4 Close V4 and close nitrogen purge.
4.3.4.5 Close V2.
4.3.4.6 Open V1 and V3.
4.3.4.7 Open V2, and, controlling flow rate at 1 L/min.,
take care not to over-pressurize system.
4.3.4.8 Continue flow through scrubber train #1 until
scale shows that approximately 100 grams of HCl have
been purged.
SEMI C3.35-1101 © SEMI 1988, 20013
4.3.4.9 Open V4 and close V3. Record the weight of
HCl cylinder.
4.3.4.10 Collect 100 grams of HCl in scrubber train #2.
Close V1 and record weight of HCl sampled.
4.3.4.11 Open nitrogen purge and purge lines, scrubber
train #1 and scrubber train #2, before disconnecting
scrubbers.
4.3.5 Sample Preparation
4.3.5.1 For each scrubber train, quantitatively wash
both scrubbers with DI water and add to 250 mL
volumetric flask.
4.3.5.2 Wash associated tubing of each scrubber train
with DI water and add to 250 mL volumetric flask.
4.3.5.3 Make up reagent blank of water from the same
lot of DI water used in the sampling.
4.3.6 Calibration — Make calibration standards by
serial dilution of standard iron solution traceable to
NIST.
4.3.7 Instrument Parameters — Perform analysis on an
inductively coupled plasma spectrometer employing
operating procedures suggested by manufacturer.
Correct result to ppm (wt/wt) basis on HCl used.
4.4 Nitrogen — This procedure is for the determination
of nitrogen in hydrogen chloride using a gas
chromatograph with a thermal conductivity detector.
4.4.1 Detection Limit — 1 ppm.
4.4.2 Instrument Parameters
4.4.2.1 Columns:
Column 1: Ascarite, 0.3 m (1 ft) by 9.6 mm (3/8 in)
OD ss or equivalent.
Column 2: Molecular Sieve 5A, 2.4 m (8 ft) by 6.4
mm (1/4 in) OD ss or equivalent.
4.4.2.2 Carrier Flow: 40 mL/min helium.
4.4.2.3 Temperatures:
Detector 50°C
Column Oven 40°C
4.4.2.4 Sample Volume: 10 mL.
4.4.3 Calibration Standard — 100 ppm nitrogen in
helium.
4.4.4 Operating Procedure
4.4.4.1 Inject the calibration standard using a gas
sampling valve. Record the retention time and peak
area.
4.4.4.2 Inject the sample to be tested in same manner
as the calibration standard. Record the retention time
and peak area.
4.4.4.3 Repeat Section 4.4.4.1.
4.4.4.4 Compare the average peak area of the
calibration standard with that of the hydrogen chloride
sample being tested. Calculate the concentration of
nitrogen, using the formula below. The results may not
exceed the specification in Section 2 of this Standard.
4.5 Oxygen + Argon — This procedure is for the
determination of oxygen + argon in hydrogen chloride
using a gas chromatograph with a thermal conductivity
detector.
4.5.1 Detection Limit — 1 ppm. The oxygen and argon
elute simultaneously and are therefore quantified as a
sum.
4.5.2 Instrument Parameters
4.5.2.1 Columns:
Column 1: Ascarite, 0.3 m (1 ft) by 9.6 mm (3/8 in)
OD or equivalent.
Column 2: Molecular Sieve 5A, 2.4 m (8 ft) by 6.4
mm (1/4 in) OD ss or equivalent
4.5.2.2 Carrier Flow: 40 mL/min helium.
4.5.2.3 Temperatures
: Detector 50°C
Column Oven 40°C
4.5.2.4 Sample Volume: 10 mL.
4.5.3 Calibration Standard — 1–5 ppm oxygen in
helium.
4.5.4 Operating Procedure
4.5.4.1 Inject the calibration standard into the column
using a gas sampling valve. Record the retention time
and peak area.
4.5.4.2 Inject the sample to be tested in the same
manner as the calibration standard. Record the retention
times and peak areas.
4.5.4.3 Repeat Section 4.5.4.1.
4.5.4.4 Compare the average peak area of the
calibration standard with that of the hydrogen chloride
sample being tested. Calculate the total concentration of
oxygen + argon, using the formula below. The result
may not exceed the specification in Section 2 of this
standard.
Sample Peak Are
a
Standard Peak Area
×
C
oncentrat
i
on
of Standard
=
C
oncentrat
i
on
of Sample