Background Statement for SEMI Draft Document 5476A
New Standard: TEST METHOD FOR DETERMINATION OF TOTAL
CARBON CONTENT IN SILICON POWDER BY INFRARED
ABSORPTION AFTER COMBUSTION IN AN INDUCTION FURNACE
Notice: 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.
Notice: 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.
Background Statement
Carbon content of PV silicon raw materials has an effect on the lifetime and cell efficiency of PV solar
product. Carbon content cannot be reduced in subsequent processing. It is important to control the carbon
content in PV silicon raw materials. Therefore it’s necessary to develop a standardized test method to
determine carbon content in silicon powder.
Review and Adjudication Information
Task Force Review
Committee Adjudication
Group:
PV Silicon Raw Materials TF
Date:
TBD
China PV Committee
March 20th, 2014
Time &Timezone:
TBD
TBD
Location:
TBD
Kerry Hotel, Shanghai, China
City,
State/Country:
TBD
Shanghai, China
Leader(s):
Dazhou Yan(SINOSICO)
Li He (CPVT)
Xiaoxia Liu( GCL)
Dongxu Chu(SINOSICO)
Kris Shen(SEMI China)
kshen@semi.org
Guangchun Zhang(CanadianSolar)
Jun Liu(CESI)
Standards Staff:
Kris Shen(SEMI China)
kshen@semi.org
Meeting date and time are subject to change, and additional TF review sessions may be scheduled if
necessary. Contact the task force leaders or Standards staff for
confirmation.Checkwww.semi.org/standards for the latest schedule.
If you have any questions, please contact the PV Silicon Raw Materials TF Leader.
Li He/CPVT
Tel: +86 510 88204827
E-mail: heli@wxzjs.com
+86 510 85299122
Or contact SEMI Staff, Kris Shenatkshen@semi.org
Semiconductor Equipment and Materials International
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Phone:408.943.6900, Fax: 408.943.7943
DRAFT
SEMI Draft Document 5476A
New Standard: TEST METHOD FOR DETERMINATION OF TOTAL
CARBON CONTENT IN SILICON POWDER BY INFRARED
ABSORPTION AFTER COMBUSTION IN AN INDUCTION FURNACE
1 Purpose
1.1 The purpose of this test method is to standardize analytical protocols for the determination of total carbon
content in PV silicon raw materials which will affect the lifetime and cell efficiency of PV solar products. This will
facilitate comparison of test results among worldwide laboratories used for monitoring or qualifying PV silicon raw
materials.
2 Scope
2.1 This test method can be used to analyze the total carbon content in silicon powder as the raw material for
producing solar-grade polycrystalline silicon. It may also be used for determining the total carbon content in single
and multi-crystalline silicon wafers and slugs if they were broken into small pieces or powder without contamination.
2.2 The test method is for use with commercially available carbon analyzers which are based on combustion in an
induction furnace principle and use infrared detector as the measuring technique.
2.3 The detection range of the method described is between 0.001 % (m/m) and 1.0 % (m/m ).
2.4 Some impurities or carbon from a lower grade accelerator can affect the accuracy of analysis data. It is
recommended to use only high purity accelerator.
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 Limitations
3.1 Not all the information needed to determine the carbon content in PV silicon raw materials is included in this
test method. For instance, determination of the optimum temperatures for measuring the carbon content in a variety
of silicon samples is not described in this test method.
3.2 The limit of detection is determined by the instrumental blank value limitations, and may vary with
instrumentation and preparation techniques.
4 Referenced Standards and Documents
4.1 SEMI Standards and Safety Guidelines
SEMI PV17 — Specification for Virgin Silicon Feedstock Materials for Photovoltaic Applications
4.2 ASTM Standards1
ASTM E50 — Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of
Metals, Ores, and Related Materials
ASTM E122 — Standard Practice for Calculating Sample Size to Estimate, With Specified Precision, the Average
for a Characteristic of a Lot or Process
ASTM E135 — Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
4.3 ISO Standard2
1
American Society for Testing and Materials, 100 Barr Harbor Drive, West Conshohocken, PA19428-2959, USA; Telephone: 610.832.9585,
Fax: 610.832.9555, http://www.astm.org
2
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, http://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 or Safety Guideline.
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
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LETTER (YELLOW) BALLOT
Document Number: 5476A
Date: 2/9/2016
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Phone:408.943.6900, Fax: 408.943.7943
DRAFT
BS EN ISO 9556 —Steel and iron—Determination of the total carbon content — Infrared absorption method after
combustion in an induction furnace
ISO 5725-2:1994—Accuracy (trueness and precision) of measurement methods and results -- Part 2: Basic method
for the determination of repeatability and reproducibility of a standard measurement method
NOTICE: Unless otherwise indicated, all documents cited shall be the latest published versions.
5 Terminology
5.1 Terminology in this test method is consistent with Terminology in ASTM E135. Required terminology specific
to this test method, not covered in ASTM E135, is indicated in ¶ 5.2.
5.2 Definitions
5.2.1 Silicon Powder — the designation is given to silicon solid materials in accordance to SEMI PV17.
5.2.2 Reference Material — material accepted as suitable for use as a calibration/sensitivity reference standard by
all parties concerned with the analyses.
5.2.3 Carbon Steel Reference Material — carbon steel sample known carbon content (%, m/m) with certification.
5.2.4 Test Sample — material (silicon) to be analyzed for carbon content by this method. Generally the test sample
is selected from a large batch of silicon raw materials and is intended to be representative of the batch.
5.2.5 Test Portion — a portion of the test sample to be tested for carbon content by this method.
6 Summary of Test Method
6.1 The principle of test method is the same with the standard BS EN ISO 9556.
6.2 Combustion — Combustion of a test portion with accelerator at a high temperature in a high-frequency
induction furnace in a current of pure oxygen.
6.3 Transformation — Transformation of carbon into carbon dioxide and/or carbon monoxide.
6.4 Measurement — Measurement by infrared absorption of the carbon dioxide and/or carbon monoxide carried by
a current of oxygen.
7 Apparatus
7.1 High-Frequency Induction Furnace and Infrared Carbon Analyzer
7.2 Electronic Balance(s) — 0.1 mg accuracy for weighing test portion, carbon steel reference materials and
accelerators; 0.01 mg accuracy for weighing anhydrous sodium carbonate in¶ 12.2.3.1
7.3 Micropipette — 100 μl, limit of error shall be less than 1 μl.
7.4 Tin Capsule — About 6 mm in diameter, 13 mm ~ 18 mm in height, 0.4 ml in volume, of known low carbon
content less than 0.0005 % (m/m).
7.5 Ceramic Crucible — Capable of withstanding combustion in an induction furnace. Ignite crucibles in an electric
furnace in air or in a current of oxygen for not less than 2 h at 1000 ℃ and store in a desiccator before use.
8 Reagents and Materials
8.1 Water free from Carbon Dioxide — Boil water for 30 min, insert a rubber stopper equipped with a soda-lime
drying tube into the neck of the flask bottle, cool to room temperature and bubble with oxygen (¶ 8.2 ) for 15 min.
Prepare just before use.
8.2 Oxygen — 99.5 % (m/m) minimum.
8.3 Pure Iron — Of known low carbon content less than 0.0005 % (m/m).
8.4 Anhydrous Sodium Carbonate — Reference Material. Dry anhydrous sodium carbonate (minimum assay :
99.9%) at 285 ℃ ±5 ℃ for 2 h and cool in a desiccator before use.
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 or Safety Guideline.
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
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LETTER (YELLOW) BALLOT
Document Number: 5476A
Date: 2/9/2016
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DRAFT
8.5 Sodium Carbonate standard Solution — Reference Material Solution, corresponding to 2.50 mg of carbon per
milliliter. Weight, to the nearest 0.1 mg, 5.5152 g of anhydrous sodium carbonate (¶ 8.4 ), dissolve in about 200 ml
of water free from carbon dioxide (¶ 8.1 ), transfer to a 250 ml one-mark volumetric flask quantitatively, dilute to
the mark with water free from carbon dioxide (¶ 8.1 )and mix.
8.6 Tin Accelerator — High-purity tin powder specified for carbon/sulfur analysis, minimum assay: 99.8 %, known
carbon content less than 0.0005 % (m/m).
8.7 Tungsten Accelerator — Minimum assay: 99.9 %, particle size from 0.42 mm to 0.85 mm (40 ASTM mesh to
20 ASTM mesh), known carbon content less than 0.0001 % (m/m).
8.8 Iron-Tungsten-Tin Mixture Accelerator — Known carbon content less than 0.0003 % (m/m).
8.9 Carbon Steel Reference Materials Series — Known carbon contents covering from 0.001 % (m/m) to 1.0 %
(m/m).
9 Sampling
9.1 No general sampling procedure is included as part of this test method, because the most suitable sampling plan
will vary considerably depending upon individual conditions.
9.2 For referee purposes, a sampling plan shall be agreed upon before conducting the test. See ASTM E122 for
suggested choices of sampling plans.
NOTE 1: The test sample to be analyzed is intended to be representative of the status of silicon powder being put into production
and it should not be contaminated in sampling procedure. If the test sample may be contaminated it should be cleaned with
appropriate cleaning agent such as anhydrous ethanol or isopropyl alcohol before being analyzed.
10 Safety Precautions
10.1 It is assumed that trained laboratory personnel are performing the analysis described under this test method
that is familiar with general laboratory safety procedures.
10.2 The risks related to combustion analysis are mainly burns in pre-igniting the ceramic crucibles and in the
fusions. Use crucible tongs at all times and suitable containers for the used crucibles. Normal precautions for
handling oxygen cylinders shall be taken. Oxygen from the combustion process should be removed effectively from
the apparatus since a high concentration of oxygen in a confined space can present a fire hazard.
10.3 Other safety care in the test process, see ASTM E50.
11 Preparation of Apparatus
11.1 The instrument shall be prepared for operation in accordance with the instrument manufacturer’s instructions.
11.2 A minimum of three warm-up specimens are analyzed prior to calibrating the instrument in order to ensure that
there are no leaks in the system and the instrument is ready for measurements.
12 Calibration and Standardization
12.1 Blank Test —Prior to the determination, carry out the following blank tests in duplicate.
12.1.1 Blank Specimen
12.1.1.1 Blank Specimen Using Tin Capsule —Weigh the mass mtc (in grams) of one tin capsule (¶ 7.4 ). Transfer it
to the ceramic crucible (¶ 7.5), press the tin capsule lightly against the bottom of the ceramic crucible, add (0.4 –
mtc)gram of the tin accelerator (¶ 8.6 ), 0.3 gram of the pure iron (¶ 8.3 ), and cover with 1.5 grams of the tungsten
accelerator (¶ 8.7 ).
12.1.1.2 Blank Specimen Without Using Tin Capsule—Add 0.4 gram of the tin accelerator (¶ 8.6 ), 0.3 gram of the
pure iron (¶ 8.3 ), and cover with 1.5 grams of the tungsten accelerator (¶ 8.7 ), or add 1.8 grams of the irontungsten-tin mixture accelerator (¶ 8.8 ), to the ceramic crucible (¶ 7.5).
NOTE 2: The quantity of accelerator will depend on the individual characteristics of the instrument and the type of material
being analyzed. The amount of accelerators should be sufficient for complete combustion.
12.1.2 Treat the crucible and contents — As specified in ¶¶ 13.2 and 13.3 .
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 or Safety Guideline.
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Document Number: 5476A
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DRAFT
12.1.3 The Reading of the Blank Tests
12.1.3.1 Case Using Sodium Carbonate for Calibration Graph — Obtain the reading of the blank tests and convert
it to milligrams of carbon by means of the calibration graph (¶¶12.2.1,12.2.2,12.2.3).
NOTE 3: The mean blank value and the difference between the two blank values should both not exceed 0.001 mg of carbon for
samples with carbon contents between 0.001 % (m/m) and 0.01 % (m/m), and 0.005 mg for samples with carbon contents
between 0.01 % (m/m) and 1.0 % (m/m), respectively. If these values are abnormally high, invest and eliminate the source of
contamination.
12.1.3.2 Case Using Carbon Steel Reference Materials for Calibration Graph — Obtain the reading of the blank
tests in the form of mass content of carbon (%, m/m) by means of the calibration graph (¶ 12.2.4 ).
NOTE 4: The mean blank value and the difference between the two blank values of carbon content should both not exceed
0.0005 % (m/m) for samples with carbon contents between 0.001 % (m/m) and 0.01 % (m/m), and 0.003 % (m/m) for samples
with carbon contents between 0.01 % (m/m) and 1.0 % (m/m), respectively. If these values are abnormally high, invest and
eliminate the source of contamination.
12.1.4 The mean blank value ( m1 ) is calculated from the two blank values.
12.2 Preparation of the Calibration Series
12.2.1 Case Using Sodium Carbonate for Calibration Graph — Samples having carbon contents between 0.001 %
(m/m) and 0.01 % (m/m).
12.2.1.1 Transfer the volumes of sodium carbonate standard solution (¶ 8.5 ) indicated in Table 1 to five 100 ml
one-mark volumetric flasks. Dilute to the mark with water free from carbon dioxide (¶ 8.1 ) and mix. Using the
micropipette (¶ 7.3 ), transfer 100 μl of each of the diluted solutions to five tin capsules (¶ 7.4 ) and dry at 50 oC for
2 h. Cool to room temperature in a desiccator.
Table 1 Calibration Graph for Samples having carbon contents between 0.001 % (m/m) and 0.01 % (m/m)
Volume Of The Standard
Solution (¶ 8.5 )
Mass Of Carbon In The Diluted
Solution, Per Milliliter
Mass Of Carbon Taken
In The Tin Capsule
Carbon Content In The Test
Portion
ml
mg
mg
% (m/m)
0#1
0
0
0
0.60
0.015
0.0015
0.001
1.20
0.030
0.0030
0.002
3.00
0.075
0.0075
0.005
6.00
0.150
0.0150
0.010
member preparation: using the micropipette (¶ 7.3 ), transfer 100 μl of water free from carbon dioxide (¶ 8.1 ) to one tin capsule (¶ 7.4 )
and dry at 50 oC for 2 h.
#1 Zero
12.2.2 Case Using Sodium Carbonate for Calibration Graph — Samples having carbon contents between 0.01 %
(m/m) and 0.1 % (m/m).
12.2.2.1 Transfer the volumes of sodium carbonate standard solution (¶ 8.5) indicated in Table 2 to five 25 ml onemark volumetric flasks. Dilute to the mark with water free from carbon dioxide (¶ 8.1 ) and mix. Using the
micropipette (¶ 7.3 ), transfer 100 μl of each of the diluted solutions to five tin capsules (¶ 7.4 ) and dry at 50 oC for
2 h. Cool to room temperature in a desiccator.
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 or Safety Guideline.
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
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LETTER (YELLOW) BALLOT
Document Number: 5476A
Date: 2/9/2016
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DRAFT
Table 2 Calibration Graph for Samples having carbon contents between 0.01 % (m/m) and 0.1 % (m/m)
Volume Of The Standard
Solution (¶ 8.5 )
Mass Of Carbon In The Diluted
Solution, Per Milliliter
Mass Of Carbon Taken
In The Tin Capsule
Carbon Content In The Test
Portion
ml
mg
mg
% (m/m)
0#1
0
0
0
1.50
0.15
0.015
0.010
3.00
0.30
0.030
0.020
7.50
0.75
0.075
0.050
15.0
1.50
0.150
0.100
Zero member preparation: using the micropipette (¶ 7.3 ), transfer 100 μl of water free from carbon dioxide (¶ 8.1 ) to one tin capsule (¶ 7.4 )
and dry at 50 oC for 2 h.
#1
12.2.3 Case Using Sodium Carbonate for Calibration Graph —Samples having carbon contents between 0.1 %
(m/m) and 1.0 % (m/m).
12.2.3.1 Weigh the anhydrous sodium carbonate (¶ 8.4 ) to the nearest 0.01 mg, and transfer to five tin capsules (¶
7.4 ), according to Table 3. The anhydrous sodium carbonate can also be transferred directly to the ceramic crucibles
(¶ 7.5) without using tin capsules.
Table 3 Calibration Graph for Samples having carbon contents between 0.1 % (m/m) and 1.0 % (m/m)
#1
Mass Of The Reference Material Anhydrous
Sodium Carbonate (¶ 8.4 )
Mass Of Carbon Taken In The Tin
Capsule Or Directly In The Crucible
Carbon Content in the Test
Portion
mg
mg
% (m/m)
0#1
0
0
1.32
0.15
0.10
2.64
0.30
0.20
6.60
0.75
0.50
13.23
1.50
1.00
Zero member
12.2.4 Case Using Carbon Steel Reference Materials for Calibration Graph
12.2.4.1 Depending on the carbon contents of the test samples, three calibration graphs, in mass fraction ranges of
0.001 % ~ 0.01 %, 0.01 % ~ 0.10 % and 0.1 % ~ 1.0 %, shall be plotted respectively. In each range, four carbon
steel reference materials (¶ 8.9 ) are required with the gradient distribution of carbon contents similar as in Table 1 ~
Table 3. The zero member of calibration graph is specified in ¶ 12.1.1.2 .
12.3 Adding Reference Materials
12.3.1 Case Using Tin Capsule（See ¶¶ 12.2.1,12.2.2,12.2.3）— Refer to the blank specimen in ¶ 12.1.1.1 , but
replace the blank tin capsules with those treated with sodium carbonate in ¶¶ 12.2.1 , 12.2.2 and 12.2.3
12.3.2 Case without Using Tin Capsules（See ¶¶ 12.2.3,12.2.4） —Refer to the blank specimen in ¶ 12.1.1.2 ,
firstly add 0.4 gram of the tin accelerator (¶ 8.6 ) and 0.3 gram of the pure iron (¶ 8.3 ), secondly add the anhydrous
sodium carbonate (¶ 8.4 ) in accordance with Table 3 or 0.150 gram (to the nearest 0.1 mg) of the carbon steel
reference material (¶ 8.9 ), finally cover with 1.5 grams of the tungsten accelerator (¶ 8.7 ), or firstly add the
anhydrous sodium carbonate (¶ 8.4 ) or the carbon steel reference material (¶ 8.9 ) and then cover with 1.8 grams of
the iron-tungsten-tin mixture accelerator (¶ 8.8 ), to the ceramic crucible (¶ 7.5).
12.4 Treatment and Measurement —Treat the crucible and contents as specified in ¶¶13.2 and 13.3
12.5 Plotting the Calibration Graph —Obtain the net reading by subtracting the reading of the zero member from
that of each member of the calibration series. Prepare a calibration graph by plotting the net reading against
milligrams or mass fraction of carbon for each member of the calibration series.
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 or Safety Guideline.
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
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LETTER (YELLOW) BALLOT
Document Number: 5476A
Date: 2/9/2016
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DRAFT
13 Sample Testing Procedure
13.1 Adding Test Portion—Weigh, to the nearest 0.1 mg, approximately 0.15 g of the test sample. The order of
adding the test portion and the accelerators is the same as ¶ 12.3
13.2 Place the ceramic crucible and contents on the pedestal post, raise to the combustion position and lock the
system. Operate the furnace in accordance with the manufacture’s instructions.
13.3 At the end of combustion and measuring cycle, remove and discard the crucible, and record the analyzer
reading.
NOTE 5: If available, use Silicon Reference Materials (Certified Reference Material) to verify the accuracy of the method.
NOTE 6: It is suggested to check out the validity of analysis process at regular intervals with Quality Control Silicon Sample
(known carbon content by no less than 11 determinations and the uncertainty of test result being evaluated).
14 Calculations
14.1 Case Using Sodium Carbonate For Calibration Graph —Convert the analyzer reading of the test portion to
milligrams of carbon (m0) by means of the calibration graph (¶¶12.2.1,12.2.2,12.2.3). The carbon content, expressed
as a percentage by mass, wc (%), is given by the equation:
wc 
m0  m1   100  m0  m1 
m  103
(1)
10m
where
m0 is the mass, expressed in milligrams of carbon, in the test portion (¶ 13.1 )
m1 is the mass, expressed in milligrams of carbon, in the blank test (¶ 12.1 )
m is the mass, in grams, of the test portion (¶ 13.1 )
14.2 Case Using Carbon Steel Reference Materials for Calibration Graph — The carbon content of the test portion,
expressed as a percentage by mass, wc (%), is given by subtracting the mean blank value ¶ 12.1.1.2 in % (m/m) from
the reading by means of the calibration graph ¶ 12.2.4 in% (m/m).
15 Report
15.1 The results to be reported — adopt the arithmetic mean of the parallel determination of the results, results
retain no less than three effective digitals.
16 Precision
16.1 A planned trial of this method was carried out by 5 laboratories, at 3 levels of carbon, each laboratory making
2 to 5 determinations of carbon content at each level. The average results obtained are listed in table 4. The results
obtained were treated statistically in accordance with ISO 5725-2. The data obtained are summarized in table 5.
Table 4 The average results, % (m/m)
Lab. 1
sample 1
0.00436
sample 2
0.0149
sample 3
0.137
Lab. 2
0.00489
0.0128
0.151
Lab. 3
0.00644
0.0169
0.139
Lab. 4
0.00466
0.0137
0.152
Lab. 5
0.00472
0.0146
0.145
Table 5 The standard deviation
Level, m
0.00502
Repeatability standard deviation, sr
0.00110
Reproducibility standard deviation, sR
0.00122
0.0144
0.0013
0.0020
0.145
0.007
0.008
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Document Number: 5476A
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DRAFT
NOTICE: Semiconductor Equipment and Materials International (SEMI) makes no warranties or representations as
to the suitability of the Standards and Safety Guidelines set forth herein for any particular application. The
determination of the suitability of the Standard or Safety Guideline 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. Standards and Safety Guidelines are subject to change
without notice.
By publication of this Standard or Safety Guideline, SEMI takes no position respecting the validity of any patent
rights or copyrights asserted in connection with any items mentioned in this Standard or Safety Guideline. Users of
this Standard or Safety Guideline 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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