Background Statement for Ratification Ballot of SEMI Draft Document 5495

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Background Statement for Ratification Ballot of 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.

Notice: This document was approved with additional technical change during adjudication of Letter Ballot # 5495 by the European Chapter of the Liquid Chemicals Global Technical Committee during its meeting on 10/6/2015. This Ratification Ballot is issued in order to satisfy the conditions for Letter Ballot approval by the Liquid Chemicals Global Technical Committee in accordance with § 9.7.2 of the Regulations. If the Ratification Ballot voting response meets the minimum acceptance conditions per Regulations § 10, then it will be automatically published.

One copy of the revised Draft Document is included to show the intended final published version. Only these proposed additional technical changes are shown in the other copy of the Draft Document with revision markups showing these intended changes, as an aid to the voter. Additions are indicated by underline and deletions are indicated by strikethrough.

Contents for vote are limited to only considering these proposed additional technical changes. All content for a new Standard and Safety Guideline or all proposed technical and editorial changes for revisions of Standards and Safety Guidelines that were included in the original Letter Ballot and passed TC Chapter review, including the ones passed with editorial changes, are incorporated, without revision markups, in both copies. All other editorial changes, if any, made and approved during the TC Chapter review are incorporated also, without revision markups, in both copies.

Background

The following is the complete list of the new proposed technical change(s) with their justifications:

Technical Changes:

¶ 2.1: Replace “grades” with “tiers”
Justification: Keep terminology consistent throughout document
Table 1: Replace
”1.450(20 °C)” with “1.450 at 20 °C”,
“0.9478 g/cm3 (20°C)” with “0.9478 g/cm3 at 20°C”,
“156 °C / 312.17 °F at 1013 hPa” with “156 °C (312.17 °F)at 1013 hPa”
“-47 °C / -53 °F” with “-47 °C (-53 °F)”,
“8.6 g/100mL (20°C) “ with “8.6 g/100mL at 20°C“, and
“44°C / 111°F” with “44°C (111°F)”
Justification: Compliance with Style Manual
¶ 12.2.1: Change “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.” to “Analyze the sample by gas chromatography (see SEMI C1, in section “Assay by Wide Bore Column Gas Chromatography), using the parameters cited in Table 2.”
Justification: Clarity
¶ 12.3.2: Change “Weigh accurately the sample volume (1.5 +/- 0.001 g) using an analytical balance.” to “Weigh accurately (+/- 0.001 g) approximately 1.5 g of sample using an analytical balance.”
Justification: Clarity
¶ 12.3.3 Change “till” to “until”
Justification: Clarity
¶ 12.8: Change “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).“ to “Trace metals analysis —Determine trace metals impurities using either Inductively coupled plasma optical emission spectroscopy (ICP-OES) or Inductively coupled plasma mass spectroscopy (ICP-MS). “
Justification: Clarity
¶ 12.9: Change “would typically be” to “is typically”
Justification: Clarity

Ballot Adjudication Information

Task Force Review / Committee Adjudication
Group: / Solvents in Advanced Processes / Joint EU Gas & Liquid Chemicals TC Chapter
Date: / October 26, 2016 / October 6, 2016
Time & Timezone: / 10am – 12 pm, CET / 2pm-5pm, CET
Location: / SEMICON Europa / SEMICON Europa
City, Country: / Grenoble, France / Grenoble, France
Leader(s): / Jean-Marie Collard (Solvay)
/ Jean-Marie Collard (Solvay)

Standards Staff: / James Amano, / James Amano,

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

*Copy with Technical Change Markup*

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 coversgrades tiers 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 / C6H10O
Molecular weight / 98.15g/mol
CAS number / 108-94-1
Refractive Index (nD) / 1.450 (at 20°C)
Density / 0.9478 g/cm3 (at 20°C)
Boiling point / 156 °C / (312.17 °F)(at 1013 hPa)
Melting point / -47°C / (-53 °F)
Solubility in water / 8.6 g/100mL (at 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), using . Tthe parameters cited in Table 2 have given satisfactory results.

Table 2Chromatography Conditions for Column Type RTX-200 or Similar

Injector Temperature / 250°C
Detector 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) approximately 1.5 g of sample using an analytical balance.

12.3.3 Inject the sample through the septum and start the automatic titration untill 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 dDetermininge 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 is 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/A
Tier 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.

SEMI Draft Document 5495

New Standard : Guide for Cyclohexanone

*Copy of Intended Final Version*

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 tiers of Cyclohexanone which are used in the semiconductor industry

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 / C6H10O
Molecular weight / 98.15g/mol
CAS number / 108-94-1
Refractive Index (nD) / 1.450 at 20°C
Density / 0.9478 g/cm3 at 20°C
Boiling point / 156 °C (312.17 °F)at 1013 hPa
Melting point / -47°C (-53 °F)
Solubility in water / 8.6 g/100mL at 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

12.2 Assay

12.2.1 Analyze the sample by gas chromatography (see SEMI C1, in section “Assay by Wide Bore Column Gas Chromatography), using the parameters cited in Table 2.

Table 2Chromatography Conditions for Column Type RTX-200 or Similar

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 (+/- 0.001 g) approximately 1.5 g of sample using an analytical balance.

12.3.3 Inject the sample through the septum and start the automatic titration until the equilibrium end-point.

ppm Acidity (CH3COOH) = Volume of NaOH (mL) x Normality of NaOH (mole/L) x 60,000

Mass of sample (g)

12.8 Trace metals analysis —Determine trace metals impurities 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.

12.9 Particles — Particle measurement method is typically Optical Particle Counter (OPC).

13 Tier B Procedures

13.2 Assay — See §12.2

13.3 Water —See §12.3

13.4 Residue After Evaporation —See §12.4