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Background Statement for SEMI Draft Document 5495
New Standard: Guide for Cyclohexanone
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.
1 Introduction:
Recent progress in semi-conductor manufacturing technology has lead to the introduction of a broad range of solvents into wet processing. Therefore, there are now solvents currently being used for which there are no SEMI guides or standards.
The Solvents in Advanced Processes Task Force held its first meeting in Berlin in 2009 to identify new solvents currently being used and to draft guides for these solvents.
2 Steps taken:
With input from ITRS representatives, semiconductor manufacturers and solvents producers The Solvents in Advanced Processes Task Force initially examined which solvents are currently being used, for which there are no SEMI guides. The task force also examined the properties of these solvents that are important for the process and whether these could be included in a guide. The Solvents in Advanced Processes Task Force then selected a couple of solvents to focus on initially with the aim of producing guides. Cyclohexanone was identified as one of those solvents needing standardization. An initial draft of the guide was produced based on task force discussions. That draft is the subject of the current ballot.
Ballot Adjudication Information
Task Force Review / Committee AdjudicationGroup: / Solvents in Advanced Processes / Joint EU Gas & Liquid Chemicals TC Chapter
Date: / October 6, 2015 / October 6, 2015
Time & Timezone: / 10am – 12 pm, CET / 2pm-5pm, CET
Location: / Messe Dresden / Messe Dresden
City, Country: / Dresden, Germany / Dresden, Germany
Leader(s): / Jean-Marie Collard (Solvay)
/ Jean-Marie Collard (Solvay)
Standards Staff: / Andrea Busch, / Andrea Busch,
This meeting’s details are subject to change, and additional review sessions may be scheduled if necessary. Contact the task force leaders or Standards staff for confirmation.
Telephone and web information will be distributed to interested parties as the meeting date approaches. If you will not be able to attend these meetings in person, but would like to participate by telephone/web, please contact Standards staff.
Check on calendar of event for the latest meeting schedule.
SEMI Draft Document 5495
New Standard : Guide for Cyclohexanone
1 Purpose
1.1 The purpose of this document is to providea guide for Cyclohexanone for which a need has been identified.
2 Scope
2.1 The scope of this document covers grades of Cyclohexanone which are used in the semiconductor industry
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 None
4 Referenced Standards and Documents
4.1 SEMI Standards and Safety Guidelines
SEMI C1 Guide for the Analysis of Liquid Chemicals
NOTICE: Unless otherwise indicated, all documents cited shall be the latest published versions.
5 Terminology
5.1 Synonyms
5.1.1 Cylohexanone, Anon, Pimelinketon
6 Properties
Table 1Properties of Cyclohexanone
Molecular formula / C6H10OMolecular weight / 98.15g/mol
CAS number / 108-94-1
Refractive Index (nD) / 1.450 (20°C)
Density / 0.9478 g/cm3 (20°C)
Boiling point / 156 °C / 312.17 °F (1013 hPa)
Melting point / -47°C / -53 °F
Solubility in water / 8.6 g/100mL (20°C)
Flashpoint / 44°C / 111°F
Appearance / Colorless Liquid with a smell of peppermint
7 Suggested Values
7.1 The suggested values for Cyclohexanone for Tier A and B are listed in Table 3.
8 Grade 1 Procedures
8.1 This section does not apply to this chemical.
9 Grade 2 Procedures
9.1 This section does not apply to this chemical.
10 Grade 3 Procedures
10.1 This section does not apply to this chemical.
11 Grade 4 Procedures
11.1 This section does not apply to this chemical.
12 Tier A Procedures
12.1 Standardized test methods are being developed for all parameters at the purity level indicated. Until standardized test methods are published, test methodology should be determined by user and producer. The Global Liquid Chemicals Committee considers a method to be valid only if method validation according to SEMI C1 has been demonstrated
12.2 Assay
12.2.1 Analyze the sample by gas chromatography (see SEMI C1, in section “Assay by Wide Bore Column Gas Chromatography). The parameters cited in Table 2 have given satisfactory results.
Table 2Chromatography Conditions for Column Type RTX-200 or Similar
Injector Temperature / 250°CDetector temperature / 280°C
Furnace temperature / 50°C, ramp up by 6°C/min to 250°C starting after 4 minutes
column / Rtx-200
Dimension: 60m x 0.32mm ID 1.5µm
Split 1:100
Sample size / 1 µL
Carrier gas / 1mL/min Helium
Detector / WFID (Flame ionisation detector)
12.3 Water — Analysis performed by coulometric Karl Fisher titration with the use of the appropriate anodic and cathodic coulometric reagents.
12.3.1 Prior to start the analysis, verify the cleanliness of the cell and prevent any exposure of the system to the humidity of the air.
12.3.2 Weigh accurately the sample volume (1.5 +/- 0.001 g) using an analytical balance.
12.3.3 Inject the sample through the septum and start the automatic titration till the equilibrium end-point.
12.4 Residue After Evaporation— Weigh accurately ~ 50 g of sample in a quartz crucible, evaporatecompletely under Nitrogen flow, cool in a desiccator, and weigh (see SEMI C1, Determination of Residue after Evaporation).
12.5 Acidity— To 50 grams of sample in a 250 mL conical flask, add 25 mL of methanol and 0.5 mL of phenolphthalein indicator solution (see SEMI C1). Titrate with 0.1 N methanolic sodium hydroxide solution until a slight pink color persists for at least 15 seconds.
ppm Acidity (CH3COOH) = Volume of NaOH (mL) x Normality of NaOH (mole/L) x 60,000
Mass of sample (g)
12.6 Chloride — The analysis is performed by Ion Chromatography equipped with a guard reversed phase cartridge, a guard column and followed by the analytical anion exchange solvent resistant column with a conductivity detector. The eluent is carbonate / bicarbonate solution. The sample is diluted with DI water (1:4) and the calibration is performed with a NIST traceable chloride standard in water
12.7 Phosphate — The analysis is performed by Ion Chromatography equipped with a guard reversed phase cartridge, a guard column and followed by the analytical anion exchange solvent resistant column with a conductivity detector. The eluent is carbonate / bicarbonate solution. The sample is diluted with DI water (1:4) and the calibration is performed with a NIST traceable phosphate standard in water
12.8 Trace metals analysis — The following method has given satisfactory results in determining trace metals impurities for the trace metals as specified using either Inductively coupled plasma optical emission spectroscopy (ICP-OES) or Inductively coupled plasma mass spectroscopy (ICP-MS).
12.8.1 The sample preparation is performed by evaporation in a closed PTFE recipient under an inert gas stream.
12.8.2 20 grams of sample are weighed in the recipient and heated on a hot plate at 180°C till nearly dryness. The residue is digested with 2 mL of an HNO3/HCl (10:1) acid solution (hot plate 200°C) for a short amount of time then diluted with DI water and cooled down. To avoid mass interferences when using ICP-MS for determination, make sure to remove all excess Chloride during dissolution process.
12.8.3 It is recommended to run each sample in duplicate. In addition prepare a sample preparation blank for each analysis. It is also recommended to use an internal standard or a spiked sample solution to correct for any matrix effect.
12.9 Particles—Particle measurement method would typically be Optical Particle Counter (OPC).
13 Tier B Procedures
13.1 Standardized test methods are being developed for all parameters at the purity level indicated. Until standardized test methods are published, test methodology shall be determined by user and producer. The Global Liquid Chemicals Committee considers a method to be valid only if method validation according to SEMI C1 has been demonstrated
13.2 Assay — See §12.2
13.3 Water —See §12.3
13.4 Residue After Evaporation —See §12.4
13.5 Acidity —See §12.5
13.6 Chloride —See §12.6
13.7 Phosphate —See §12.7
13.8 Trace metals analysis —See §12.8
13.9 Particles— See §12.9
14 Tier C Procedures
14.1 This section does not apply to this chemical.
15 Tier D Procedures
15.1 This section does not apply to this chemical.
Table 3Suggested Values for Cyclohexanone
Previous SEMI Reference # / N/A / N/ATier A / Tier B
(Guide) / (Guide)
Assay (Cyclohexanone) / ≥99.5% / ≥99.5%
Water / 0.1% max. / 0.08% max.
Residue After Evaporation / 50 ppm max. / 10 ppm max.
Free Acid
(as CH3COOH) / 10 ppm max. / 10 ppm max.
Chloride / 1 ppm max. / 0.2 ppm max.
Phosphate / 1 ppm max. / 0.5 ppm max.
Aluminum (Al) / 10 ppb max. / 1 ppb max.
Antimony (Sb) / -- / --
Arsenic (As) / -- / --
Barium (Ba) / 10 ppb max. / 1 ppb max.
Boron (B) / 10 ppb max. / 1 ppb max.
Cadmium (Cd) / -- / --
Calcium (Ca) / 10 ppb max. / 1 ppb max.
Chromium (Cr) / 10 ppb max. / 1 ppb max.
Cobalt (Co) / 10 ppb max. / 1 ppb max.
Copper (Cu) / 10 ppb max. / 1 ppb max.
Iron (Fe) / 10 ppb max. / 1 ppb max.
Lead (Pb) / 10 ppb max. / 1 ppb max.
Lithium (Li) / 10 ppb max. / 1 ppb max.
Magnesium (Mg) / 10 ppb max. / 1 ppb max.
Manganese (Mg) / 10 ppb max. / 1 ppb max.
Nickel (Ni) / 10 ppb max. / 1 ppb max.
Potassium (K) / 10 ppb max. / 1 ppb max.
Sodium (Na) / 10 ppb max. / 1 ppb max.
Tin (Sn) / 10 ppb max. / 1 ppb max.
Titanium (Ti) / 10 ppb max. / 1 ppb max.
Vanadium (V) / -- / --
Zinc (Zn) / 10 ppb max. / 1 ppb max.
Particle (#1) > 0.2µm / 500 /mL max. / 500 /mL max.
Particle (#1) > 0.1µm / 1000 /mL max. / 1000 /mL max.
#1: bulk shipment – point of filling
NOTICE: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.
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 development) activity. All other reproduction and/or distribution without the prior written consent of SEMI is prohibited.
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