Background Statement for SEMI Draft document 4734A
NEW STANDARD: SPECIFICATION AND GUIDE FOR BORON
TRICHLORIDE (BCl3)
Note: This background statement is not part of the balloted item. It is provided solely to assist the recipient in
reaching an informed decision based on the rationale of the activity that preceded the creation of this document.
Note: Recipients of this document are invited to submit, with their comments, notification of any relevant patented
technology or copyrighted items of which they are aware and to provide supporting documentation. In this context,
“patented technology” is defined as technology for which a patent has issued or has been applied for. In the latter
case, only publicly available information on the contents of the patent application is to be provided.
The Gases Committee has been combining the common SEMI Gases into single specifications to make it
an orderly and efficient way that would facilitate ease of use or reference. The committee took
advantage of the common traits in all the existing specifications to reduce the total volume of specs and to
reinforce their commonalities.
In the past ballot cycles, the committee has successfully combined Oxygen, Hydrogen and Nitrogen gases
below
SEMI C54-1103, SPECIFICATIONS AND GUIDELINES FOR OXYGEN
SEMI C58-0305, SPECIFICATIONS AND GUIDELINES FOR HYDROGEN
SEMI C59-1103, SPECIFICATIONS AND GUIDELINES FOR NITROGEN
In a continuing process, this ballot proposal is to combine
SEMI C3.33-92 (Reapproved 0303) Standard For Boron Trichloride (BCl3) (Provisional) and
SEMI C3.51-1101 Specification For Boron Trichloride (BCl3), 99.98% Quality
In this document, the committee carried out the following steps:
First, new Purpose, Scope sections and other mandatory sections were added to the ballot. Its purpose is
to modify the titles of the combine standards for a given gases into a single stand-alone specification. This
is being accomplished as follows:
1) Collect and group all gases standards and combined into one specification for each gases that includes
all grades.
2) Combine all relevant gases tables into a single table in the consolidated specification
3) Re-designate the combined specifications with a single designation (C3.xx) for each gas.
4) Reference the previous SEMI designation numbers (C3.yy) for grades at the top of each column in the
table.
This involves reformatting the standards, updating any technical information, format according to SEMI
editorial guidelines, and obtaining approval of the committee by balloting.
NOTE:
If this ballot is approved, SEMI C3.33 and C3.51 will be submitted for withdrawal in
subsequent meeting.
The results of this ballot will be reviewed and adjudicated by NA Facilities and Gases Committee during their
meetings late March 2011 in San Jose, CA. Check www.semi.org/standards for the latest meeting schedule.
For question on the ballot, contact SEMI Staff, Kevin Nguyen at knguyen@semi.org
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SEMI Draft Document 4734A
NEW STANDARD: SPECIFICATION AND GUIDE FOR BORON
TRICHLORIDE (BCl3)
1 Purpose
1.1 The purpose of this document is to provide specification and guide for boron trichloride (BCl3) that are used in
the semiconductor industry.
2 Scope
2.1 This specification relates to a geometry of 0.5 µ or less (0.35 to 0.5 range) and describes analytical techniques
using gas phase analysis.
2.2 If analytical methods are not complete, the requirements are presented as guides.
NOTICE: SEMI Standards and Safety Guidelines do not purport to address all safety issues associated with their
use. It is the responsibility of the users of the documents to establish appropriate safety and health practices, and
determine the applicability of regulatory or other limitations prior to use.
3 Description
3.1 Boron trichloride is a colorless toxic and corrosive gas at room temperature and atmospheric pressure which
fumes in the presence of moist air. It has a choking odor.
4 Referenced Standards and Documents
4.1 SEMI Standard
SEMI C3 — Specifications for Gases
4.2 ISO Standard1
ISO 6145-1 — Preparation of calibration gas mixtures – Dynamic volumetric methods – Part 1: Methods of
calibration
NOTICE: Unless otherwise indicated, all documents cited shall be the latest published versions.
5 Terminology
5.1 Terminology appropriate to this standard is defined in SEMI C3.
6 Requirements
6.1 Purity and other requirements for boron trichloride are given in Table 1.
1
International Organization for Standardization, ISO Central Secretariat, 1, rue de Varembé, Case postale 56, CH-1211 Geneva 20, Switzerland.
Telephone: 41.22.749.01.11; Fax: 41.22.733.34.30 Website: www.iso.ch
This is a draft document of the SEMI International Standards program. No material on this page is to be construed as an official or adopted standard. Permission is granted to
reproduce and/or distribute this document, in whole or in part, only within the scope of SEMI International Standards committee (document development) activity. All other
reproduction and/or distribution without the prior written consent of SEMI is prohibited.
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Table 1 Impurity and Other Requirements for Boron Trichloride
Previous SEMI Reference #
C3.51
(Specification)
C3.33
(Guide)
Grade
99.98%
(vapor phase)
99.9995%
(liquid phase)
Maximum Acceptable Level (ppm)#1
Impurities
Nitrogen (N2)
Carbon Dioxide (CO2)
Chlorine (Cl2)
Hydrogen Chloride (HCl)
Phosgene (COCl2)
Silicon Tetrachloride (SiCl4)
TOTAL LISTED IMPURITIES
(excluding metals)
Impurities
Aluminum (Al)
Calcium (Ca)
Copper (Cu)
Magnesium (Mg)
Iron (Fe)
Nickel (Ni)
Potassium (K)
Silicon (Si)
Sodium (Na)
TOTAL IMPURITIES
5
2
10
100
1
2
120
10 (vapor phase)
1 (vapor phase)
1(vapor phase)
12 (vapor phase)
0.5
0.5
1
Maximum Acceptable Level (ppm w)
0.5 (liquid phase)
0.5 (liquid phase)
0.5 (liquid phase)
0.5 (liquid phase)
0.5 (liquid phase)
0.5 (liquid phase)
0.5 (liquid phase)
1 (liquid phase)
0.5 (liquid phase)
5 (liquid phase)
#1 An analysis of significant figures has not been considered. The number of significant figures will be based on analytical accuracy and
precision of the provided procedure.
7 Properties of Boron Trichloride
Table 2 Properties of Boron Trichloride (for information only)
Molecular Formula
CAS Number
Molecular weight
Boiling point at atm
Density of gas at 20°C and 1 atm
Specific gravity
Density of liquid at –118°C
Metric Units
US Units
BCl3
10294-34-5
117.17
12.4°C
5.326 kg/m3
4.12
1372.8 kg/m3
BCl3
10294-34-5
117.17
54.3°F
0.3325 lb/ft3
4.12
85.76 lb/ft3
8 Analytical Procedures for Boron Trichloride, 99.98% Purity
NOTE 1: The boiling point of boron trichloride is 12.4°C. It is recommended that, prior to the sampling operation, the cylinder
should be allowed to reach room temperature to prevent the possibility of any suck-back.
8.1 Nitrogen — This procedure is for the determination of nitrogen in boron trichloride using a gas chromatograph
fitted with a backflush valve and a thermal conductivity detector.
8.1.1 Detection Limits — 0.5 ppm nitrogen.
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8.1.2 Instrument Parameters
8.1.2.1 Columns:


Column 1:
Column 2:
Porapak® QS 60/80 mesh 2 m (6 ft) × 3.2 mm (1/8") OD SS or equivalent.
Molecular sieve 5A 60/80 mesh 2 m (6 ft) × 3.2 mm (1/8") OD SS or equivalent. 
8.1.2.2 Carrier Gas Flow — Helium with minimum purity of 99.9999%. Flow 25 mL/min
NOTE 2: The helium carrier gas should contain less than 10 ppb of the impurities it is desired to measure. This is best achieved
by using a commercial helium gas purifier.
8.1.2.3 Sample Volume — 2.5 mL.
8.1.2.4 Temperatures:


Column Temperature:
Detector Temperature:
100°C
100°C
8.1.2.5 Bridge Current — 200 mA.
8.1.3 Calibration Standard — 1–10 ppm nitrogen in helium.
8.1.3.1 Calibration — Construct a calibration curve which contains at least three points covering the range of
interest. Verify the standards employed independently by established traceability to recognized national or
international standards.
8.1.4 Operating Procedure
8.1.4.1 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 3: Introduce the calibration standard as many times as necessary to achieve the desired precision.
8.1.4.2 Inject the sample to be tested in the same manner as the calibration standard. Record the retention time and
peak areas (see Note 1).
8.1.4.3 Repeat ¶ 8.1.4.1.
8.1.4.4 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 table 1 of this standard.
Sample Peak Area Concentration Concentration
 of S tandard  of Sample
Standard Peak Area
(1)
8.2 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.
8.2.1 Detection Limits — 0.5 ppm carbon dioxide.
8.2.2 Instrument Parameters
8.2.2.1 Columns:


Column 1:
Column 2:
Porapak® QS 60/80 mesh 3m (10 ft.) by 3.2 mm (1/8") OD SS or equivalent
Porapak® QS 60/80 mesh 2.5 m (8 ft.) by 3.2 mm (1/8") OD SS or equivalent
8.2.2.2 Carrier Gas Flow — Helium with minimum purity of 99.9999%, flow 25 mL/mm (See Note 2.)
8.2.3 Sample Volume — 2.5 mL.
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8.2.4 Temperatures:


Column Temperature:
Detector Temperature:
60°C
110°C
8.2.5 Bridge Current — 200 mA.
8.2.6 Calibration Standard — 1–5 ppm carbon dioxide in helium.
8.2.6.1 Calibration — Construct a calibration curve which contains at least three points covering the range of
interest. Verify the standards employed independently by established traceability to recognized national or
international standards.
8.2.7 Operating Procedure
8.2.7.1 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 3).
8.2.7.2 Inject the sample to be tested in the same manner as the calibration standard (see Note 1). Record the
retention time and peak areas.
8.2.7.3 Repeat ¶ 8.2.7.1.
8.2.7.4 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 Area Concentration Concentration
 of S tandard  of Sample
Standard Peak Area
(2)
8.3 Chlorine — This procedure is for the analysis of chlorine in boron trichloride using a gas chromatograph with a
thermal conductivity detector.
8.3.1 Detection Limits — 5 ppm chlorine.
8.3.2 Instrument Parameters
8.3.2.1 Column 60 m (200 ft.) 0.53 mm (1/32") ID Dimethyl silicone megabore capillary column (Ristek RTxi)
8.3.2.2 Carrier Gas — Helium with a minimum purity of 99.9999%, 25–30 mL/min (See Note 3.)
8.3.2.3 Sample Volume — 2.0 mL.
8.3.2.4 Temperatures:


Column Temperature:
Detector Temperature:
100°C
110°C
8.3.2.5 Bridge Current — 200 mA.
8.3.3 Calibration Standard — 5–10 ppm chlorine in helium.
8.3.3.1 Calibration — Construct a calibration curve which contains at least three points covering the range of
interest. Verify the standards employed independently by established traceability to recognized national or
international standards.
8.3.4 Operating Procedure
8.3.4.1 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 3).
8.3.4.2 Inject the sample to be tested in the same manner as the calibration standard. Record the retention time and
peak areas (see Note 1).
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8.3.4.3 Repeat ¶ 8.3.4.1.
8.3.4.4 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 table 1 of this standard.
Sample Peak Area Concentration Concentration
 of S tandard  of Sample
Standard Peak Area
(4)
8.4 Hydrogen Chloride, Phosgene, and Silicon Tetrachloride — This procedure is for the determination of hydrogen
chloride, phosgene, and silicon tetrachloride using a Fourier transform infrared (FTIR) analyzer.
8.4.1 Detection Limits

10 ppm hydrogen chloride

1 ppm phosgene

0.5 ppm silicon tetrachloride
8.4.2 Instrument Parameters
8.4.2.1 Cell — 16 cm × 16 mm ID K Br windows
8.4.2.2 Wavenumbers:



Hydrogen Chloride: 2970–2990 (cm-1)
Phosgene:
855–865 (cm-1)
Silicon Tetrachloride: 610–630 (cm-1)
8.4.2.3 The associated sampling system must be equipped with inert gas purging and evacuation capabilities.
8.4.3 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 4: 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.
8.4.4 Operating Procedures
8.4.4.1 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.
8.4.4.2 Fill the sample into the cell following the same procedures used in ¶ 8.4.4.1 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 table 1 of this specification.
Measured
Absorbance of
the Sample
Concentration Concentration
Measured  of S tandard  of Sample
Absorbance of
the Standard
(5)
NOTE 5: 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.
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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 6: Low-pressure plastic parts should be cleaned as follows using 18 MΩcm water:
a. Fill sampling lines with the following solutions for 30 minutes: NH4OH 25%: H2O2 35%: H2O = 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%: H2O2 35%; H2O = 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 MΩcm.
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 7: 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.
8.5 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.
8.5.1 Detection Limits
NOTE 8: Atomic absorption or inductive coupled plasma instruments may vary depending on the manufacturer. In all cases, refer
to individual instrument vendor instructions.
8.5.2 Instrument Parameters — Operate the designated analytical instruments according to the manufacturer’s
instructions.
8.5.3 Sampling Procedure
8.5.3.1 Clean all metallic and plastic components according to the procedures described in Notes 5 and 6. Use 18
MΩcm water.
8.5.3.2 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.
8.5.3.3 Connect the sampling system to the sample boron trichloride cylinder (see Note 7).
8.5.3.4 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.
8.5.3.5 While observing the sampling apparatus, operate the needle valve to admit sample slowly to the sampling
apparatus. Initial absorption will be fast.
8.5.3.6 The sample flow is halted when no further absorption seems to be taking place (i.e., when bubble rate
increases at the vent).
8.5.3.7 The argon purge is re-established for a further 15 minutes.
8.5.3.8 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.
8.5.3.9 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.
8.5.3.10 A sample of the solution is diluted × 10 with water. The aliquot is taken from the supernatant liquid.
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8.5.3.11 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.
8.5.3.12 Calibration curves are prepared using standard solutions covering the elements required. Traceable
standards can be obtained from national and international bodies.
8.5.3.13 Calculate the concentration of iron and nickel content using the calibration curve and the volume of boron
trichloride sampled.
Figure 1
Chromatogram Showing the Determination of Nitrogen in Boron Trichloride
Figure 2
Chromatogram Showing the Determination of Carbon Dioxide in Boron Trichloride
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Figure 3
Chromatogram Showing the Determination of Chlorine in Boron Trichloride
Figure 4A
Infra Red Absorption Spectra of Hydrogen Chloride in Boron Trichloride
Figure 4B
Infra Red Absorption of Phosgene in Boron Trichloride
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Figure 4C
Infra Red Absorption Spectra of Silicon Tetrachloride in Boron Trichloride
9 Analytical Procedures for Boron Trichloride, 99.9995% Purity
9.1 Analytical methods for are not complete, impurities listed in table 1 are presented as a guide.
NOTICE: SEMI makes no warranties or representations as to the suitability of the standards set forth herein for any
particular application. The determination of the suitability of the standard is solely the responsibility of the user.
Users are cautioned to refer to manufacturer’s instructions, product labels, product data sheets, and other relevant
literature respecting any materials or equipment mentioned herein. These standards are subject to change without
notice.
The user’s attention is called to the possibility that compliance with this standard may require use of copyrighted
material or of an invention covered by patent rights. By publication of this standard, SEMI takes no position
respecting the validity of any patent rights or copyrights asserted in connection with any item mentioned in this
standard. Users of this standard are expressly advised that determination of any such patent rights or copyrights, and
the risk of infringement of such rights, are entirely their own responsibility.
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