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SEMI C3.51-11 01 © SEMI 1995 , 2001 3 7.3.3 Cali bration St andard — 5–10 ppm chlo rine in heli um. 7.3.3.1 Calibratio n — Constru ct a calibration curve in the rang e of interest. Verify t he standards employed independ…

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SEMI C3.51-1101 © SEMI 1995, 2001 2
7.1.2.4 Temperatures:
Column Temperature 100°C
Detector Temperature 100°C
7.1.2.5 Bridge Current — 200 mA.
7.1.3 Calibration Standard — 1–10 ppm nitrogen in
helium.
7.1.3.1 Calibration — Construct a calibration curve in
the range of interest. Verify the standards employed
independently by established traceability to recognized
national or international standards.
7.1.4 Operating Procedure
7.1.4.1 Inject the calibration standard into the column
using a gas sampling valve. Adjust the backflush valve
operation sequence to present the nitrogen. Record the
retention time and peak area. A sample chromatogram
is shown in Figure 1.
NOTE 4: Introduce the calibration standard as many times as
necessary to achieve the desired precision.
7.1.4.2 Inject the sample to be tested in the same
manner as the calibration standard. Record the retention
time and peak areas (see Note 2).
7.1.4.3 Repeat Section 7.1.4.1.
7.1.4.4 Compare the average peak areas of the nitrogen
in the calibration standard to that of the boron
trichloride sample being tested. Calculate the
concentration of nitrogen using the formula below. The
results may not exceed the specification in Section 5 of
this standard.
Sample Pea
k
Are
a
Standard Peak Are
a
×
Concentratio
n
of Standard
=
Concentratio
n
of Sample
7.2 Carbon Dioxide — This procedure is for the
determination of carbon dioxide in boron trichloride
using a gas chromatograph fitted with a backflush and a
thermal conductivity detector.
7.2.1
Detection Limits — 0.5 ppm carbon dioxide.
7.2.2 Instrument Parameters
7.2.2.1 Columns:
Column 1 Porapak QS 60/80 mesh 3m (10 ft.) by 3.2
mm (1/8") OD SS or equivalent
Column 2 Porapak QS 60/80 mesh 2.5 m (8 ft.) by 3.2
mm (1/8") OD SS or equivalent
7.2.2.2 Carrier Gas Flow — Helium N6.0 flow 25
mL/mm (See Note 3.)
7.2.3
Sample Volume — 2.5 mL.
7.2.4
Temperatures:
Column Temperature 60°C
Detector Temperature 110°C
7.2.5 Bridge Current — 200 mA.
7.2.6 Calibration Standard — 1–5 ppm carbon dioxide
in helium.
7.2.6.1
Calibration — Construct a calibration curve in
the range of interest. Verify the standards employed
independently by established traceability to recognized
national or international standards.
7.2.7
Operating Procedure
7.2.7.1 Inject the calibration standard into the column
using a gas sampling valve. Adjust the backflush valve
operation sequence to present the carbon dioxide peak.
Record the retention time and peak area. A sample
chromatogram is shown in Figure 2 (see Note 4).
7.2.7.2
Inject the sample to be tested in the same
manner as the calibration standard (see Note 2). Record
the retention time and peak areas.
7.2.7.3
Repeat Section 7.2.7.1.
7.2.7.4 Compare the average peak areas of the carbon
dioxide in the calibration standard to that in the boron
trichloride sample being tested. Calculate the
concentration of carbon dioxide using the formula
below.
Sample Peak Are
a
Standard Peak Are
a
×
Concentratio
n
of Standard
=
Concentratio
n
of Sample
7.3 Chlorine — This procedure is for the analysis of
chlorine in boron trichloride using a gas chromatograph
with a thermal conductivity detector.
7.3.1
Detection Limits — 5 ppm chlorine.
7.3.2 Instrument Parameters
7.3.2.1 Column 60 m (200 ft.) 0.53 mm (1/32") ID
Dimethyl silicone megabore capillary column (Ristek
RTxi)
7.3.2.2
Carrier Gas — Helium: N6.0 25–30 mL/min
(See Note 3.)
7.3.2.3 Sample Volume — 2.0 mL.
7.3.2.4 Temperatures:
Column Temperature 100°C
Detector Temperature 110°C
7.3.2.5 Bridge Current — 200 mA.
SEMI C3.51-1101 © SEMI 1995, 20013
7.3.3 Calibration Standard — 5–10 ppm chlorine in
helium.
7.3.3.1 Calibration — Construct a calibration curve in
the range of interest. Verify the standards employed
independently by established traceability to recognized
national or international standards.
7.3.4
Operating Procedure
7.3.4.1 Inject the calibration standard into the column
using a gas sampling valve. Record the retention time
and peak area. A sample chromatogram is shown in
Figure 3 (see Note 4).
7.3.4.2
Inject the sample to be tested in the same
manner as the calibration standard. Record the retention
time and peak areas (see Note 2).
7.3.4.3
Repeat Section 7.3.4.1.
7.3.4.4 Compare the average peak areas of the chlorine
in the calibration standard with that obtained in the
boron trichloride sample being tested. Calculate the
concentration of chlorine using the formula below. The
results may not exceed the specification in Section 5 of
this standard.
Sample Pea
k
Are
a
Standard Peak Are
a
×
Concentratio
n
of Standard
=
Concentratio
n
of Sample
7.4 Hydrogen Chloride, Phosgene, and Silicon
Tetrachloride — This procedure is for the
determination of hydrogen chloride, phosgene, and
silicon tetrachloride using a Fourier transform infra red
(FTIR) analyzer.
7.4.1
Detection Limits
10 ppm hydrogen chloride
1 ppm phosgene
0.5 ppm silicon tetrachloride
7.4.2
Instrument Parameters
7.4.2.1 Cell Path Length — 16 cm × 16 mm ID K Br
windows
7.4.2.2 Wavenumbers:
Hydrogen Chloride 2970–2990 (cm
-1
)
Phosgene 855–865 (cm
-1
)
Silicon Tetrachloride 610–630 (cm
-1
)
7.4.2.3 The associated sampling system must be
equipped with inert gas purging and evacuation
capabilities.
7.4.3
Calibration Standards — Prepare calibration
standards for 10–100 ppm hydrogen chloride, 1–5 ppm
phosgene, and 0.5–5 ppm silicon tetrachloride in boron
trichloride.
NOTE 5: To ensure stability, the hydrogen chloride
calibration standard should be prepared dynamically using a
method defined in ISO 6145/part 1.1986. Phosgene and
silicon tetrachloride standards may be prepared by syringe
additions to liquid boron trichloride in the cooled sealed
container.
7.4.4 Operating Procedures
7.4.4.1 Evacuate and purge the sampling system
leading to the cell and purge the cell with dry nitrogen
for 30 minutes. Fill the cell with calibration standard.
Record the absorbance of hydrogen chloride, phosgene,
and silicon tetrachloride. A sample spectrum is shown
in Figures 4A, 4B, and 4C.
7.4.4.2
Fill the sample into the cell following the same
procedures used in Section 7.4.4.1 above. Record the
absorbance at the same wave number as the calibration
standard. Calculate the concentrations of hydrogen
chloride, phosgene, and silicon tetrachloride. The
results should not exceed the amount specified in
Section 3 of this specification.
Measure
d
Absorbance of
the Sample
Measured
Absorbance of
the Standard
×
Concentration
of Standard
=
Concentration
of Sample
NOTE 6: The following method should be adopted for
cleaning metallic parts used for sampling hydrogen chloride
gas:
a. Clean in a bath with methanol or isopropanol.
b. Ultrasonic clean in an appropriate solvent.
c. Rinse with isopropanol under Class 100 bench.
This cleaning method should be applied when a new cylinder
has to be connected and repeated after ten samplings, or if a
new cylinder has to be connected.
NOTE 7: Low-pressure plastic parts should be cleaned as
follows using 18 MΩcm water:
a. Fill sampling lines with the following solutions for 30
minutes: NH
4
OH 25%: H
2
O
2
35%: H
2
O = 1 to 1 to 5
parts by vol.
b. Wash sampling lines 5 times with water.
c. Fill sampling lines with the following solutions for 30
minutes: HCl 37%: H
2
O
2
35%; H
2
O = 1 to 1 to 5 parts
by vol.
d. Wash sampling lines a minimum of 5 times with water.
Terminate if the resistivity of the wash water from the
lines is more than 18 M
Ωcm.
SEMI C3.51-1101 © SEMI 1995, 2001 4
Cleaning of lines, flow meters and valves shall be completed
before a new cylinder has to be analyzed and shall be repeated
after 10 samplings, or if a new cylinder has to analyzed. The
impingers must be rinsed with water after each sampling.
Before a new cylinder has to be analyzed and after five
samplings, the impingers must be cleaned using the above
described procedures. Drying of the impingers is not
recommended (contamination risks).
NOTE 8: Cleaning of cylinder valve.
Clean outside (visible parts, threads) with wipe. Clean the
interior parts of the valve-outlet with methanol or isopropanol
using a syringe, followed by a purge with filtered gas.
7.5 Iron and Nickel — This procedure is for the
determination of iron and nickel in gas phase boron
trichloride using atomic absorption or inductive coupled
plasma methods.
7.5.1
Detection Limits
7.5.2 Instrument Parameters — Operate the designated
analytical instruments according to the manufacturer’s
instructions.
7.5.3
Sampling Procedure
7.5.3.1 Clean all metallic and plastic components
according to the procedures described in Notes 6 and 7.
Use 18 MΩcm water.
7.5.3.2
Connect all components of the sampling
system.
NOTE 9: The apparatus is charged with sufficient water to
just cover the rim of the funnel (approximately 100 ml). A
magnetic stirrer is introduced and the apparatus closed.
7.5.3.3 Connect the sampling system to the sample
boron trichloride cylinder (see Note 8).
7.5.3.4 Purge with filtered argon (< 0.01 µ) at
approximately 1 L/min. for 15 minutes prior to
sampling. During this period, the apparatus is inclined
so as to allow a higher flow rate without excessive
agitation of the water.
NOTE 10: Due to the design of the apparatus, suck-back
should be prevented, but this must be guarded against. A
bubble rate of about one per second should be set.
7.5.3.5 While observing the sampling apparatus,
operate the needle valve to admit sample slowly to the
sampling apparatus. Initial absorption will be fast.
7.5.3.6
The sample flow is halted when no further
absorption seems to be taking place (i.e., when bubble
rate increases at the vent).
7.5.3.7
The argon purge is re-established for a further
15 minutes.
7.5.3.8 The apparatus is allowed to cool and the
contents quantitatively transferred to a 250 ml
polypropylene flask.
NOTE 11: The solution prepared above will contain some
crystals of boric acid which have come out of solution during
cooling. For the purpose of analysis, the concentration of
boric acid must be reduced. Also the amount of BCl
3
samples
need to be determined.
7.5.3.9 A 5 ml aliquot of the solution is titrated against
1 M NaOH using methyl red as an indicator. The
quantity of sample boron trichloride taken is then
calculated.
7.5.3.10
A sample of the solution is diluted × 10 with
water. The aliquot is taken from the supernatant liquid.
7.5.3.11
Analysis is carried out in a suitable analyzer
capable of meeting the required detection limits. A
blank solution of 1% hydrochloric acid is used.
Yttrium is used as an internal standard at a level of 0.2
ppm added to all analysis solutions.
7.5.3.12
Calibration curves are prepared using standard
solutions covering the elements required. Traceable
standards can be obtained from national and
international bodies.
7.5.3.13
Calculate the concentration of iron and nickel
content using the calibration curve and the volume of
boron trichloride sampled.