Background Statement for SEMI Draft Document 5324 NEW STANDARD: GUIDE FOR CYCLOPENTANONE 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. 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. 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 guideline. The Solvents in Advanced Processes Task Force then selected a couple of solvents to focus on initially with the aim of producing guides. Cyclopentanone 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 Adjudication Group: EU Gases and Liquid Chemicals Committee EU Gases and Liquid Chemicals Committee Date: Tuesday, October 08, 2013 Tuesday, October 08, 2013 Time & Timezone: 14:00-17:30 CEST 14:00-17:30 CEST Location: SEMICON Europa SEMICON Europa City, State/Country: Dresden, Germany Dresden, Germany Leader(s): Jean-Marie Collard (jeanmarie.collard@solvay.com) Gummaar De Vos (gummaar_devos@fujifilm-ffem.com) Gordon Ferrier (ferrieg@airproducts.com) Jean-Marie Collard (jeanmarie.collard@solvay.com) Gummaar De Vos (gummaar_devos@fujifilm-ffem.com) Gordon Ferrier (ferrieg@airproducts.com) Standards Staff: Michael Tran 408.943.7019 / mtran@semi.org Yann Guillou +33 6 85 82 61 36 / yguillou@semi.org Michael Tran 408.943.7019 / mtran@semi.org Yann Guillou +33 6 85 82 61 36 / yguillou@semi.org This ballot and all responses to it will be adjudicated at the next meeting of the Europe Gases and Liquid Chemicals Committee, to be held in Dresden, Germany on Tuesday, October 8th, 2013 (in conjunction with SEMICON Europa
This meeting s details are subject to change, and additional review sessions may be scheduled if necessary. Contact 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.
SEMI Draft Document 5324 NEW STANDARD: GUIDE FOR CYCLOPENTANONE 1 Purpose 1.1 The purpose of this document is to provide a guide for Cyclopentanone for which a need has been identified. 2 Scope 2.1 The scope of this document covers Cyclopentanone which is 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 Referenced Standards and Documents 3.1 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. 4 Properties Table 1 Properties of Cyclopentanone Molecular formula C 5 H 8 O Molecular weight 84.12 g/mol CAS number 120-92-3 Density 0.95 g/cm 3 Boiling point 131 C (1013 hpa) Melting point -58.2 C Solubility in water Slightly soluble Flashpoint 26 C Appearance Colourless Liquid 5 Suggested Values 5.1 The suggested values for Cyclopentanone for Tier A are listed in Table 3. 6 Grade 1 Procedures 6.1 This section does not apply to this chemical. 7 Grade 2 Procedures 7.1 This section does not apply to this chemical. 8 Grade 3 Procedures 8.1 This section does not apply to this chemical. 9 Grade 4 Procedures 9.1 This section does not apply to this chemical. Page 1
10 Tier A Procedures NOTE 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 SEMI Standards Global Liquid Chemicals Committee considers a method to be valid only if method validation according to SEMI C1 has been demonstrated. 10.1 Assay Analyse the sample by gas chromatography (see SEMI C1, Assay by Wide Bore Column Gas Chromatography ). The parameters cited have given satisfactory results. 10.1.1 Column: 50 meter x 320 micron I.D. fused silica capillary coated with 100% dimethyl polysiloxane which has been surface bounded 10.1.2 Column temperature: 80 C isothermal for 3 minutes then programmed to 260 C at 20 C/min, then isothermal for 5 min. Table 2 Chromatography Conditions Injector Temperature 250 C Detector temperature 280 C Sample size 0.5 µl split ratio 1/50 Carrier gas Detector Approximate Retention Time (min): Cyclopentanone Nitrogen Flame ionisation detector (hydrogen) 6.6 10.2 Color Dilute 2.0 ml of Pt-Co stock solution (APHA 500, see SEMI C1) to 100 ml with DI water. Compare this standard (APHA 10) with 100 ml of sample in Nessler tubes. View vertically over a white background. The sample must be no darker than the standard. 10.3 Water Analysis performed by coulometric Karl Fisher titration with the use of the appropriate anodic and cathodic coulometric reagents in methanol. 10.3.1 Prior to start the analysis, verify the cleanliness of the cell and prevent any exposure of the system to the humidity of the air. 10.3.2 Weigh accurately the sample volume (0.5 +/-0.001 g) using an analytical balance. 10.3.3 Inject the sample through the septum and start the automatic titration till the equilibrium end-point. 10.4 Acidity Weigh 50 g of sample into a 150 ml beaker and record the weight. Add 50 ml of a mixture of DI water and methanol (1:1) and stir. 10.4.1 Titrate potentiometrically with standardized 0.1 N Sodium hydroxide till end-point. Volume of NaOH ( ml) Normality of Acidity meq 100 g Sample Mass ( g) 10 NaOH mol L 10.5 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). Page 2
10.5.1 The sample preparation is performed by evaporation in a closed PTFE recipient under an inert gas stream. 10.5.2 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 at 80 C with 2 ml of an HNO 3 /HF acid solution and then diluted with DI water and cooled down. 10.5.3 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. 10.6 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. 10.6.1 The sample is diluted with DI water (1:4) and the calibration is performed with a NIST traceable chloride standard in water. 11 Tier B Procedures 11.1 This section does not apply to this chemical. 12 Tier C Procedures 12.1 This section does not apply to this chemical. 13 Tier D Procedures 13.1 This section does not apply to this chemical. Table 3 Impurity Limits and Other Suggested Values for Cyclopentanone Previous SEMI Reference # N/A Tier A (Guide) Assay (Cyclopentanone) 99.5% Water 1000 ppm max Colour (APHA) 10 max Acidity 0.20 meq/100g max Chloride 200 ppb max Aluminum (Al) Antimony (Sb) -- Arsenic (As) -- Barium (Ba) -- Boron (B) -- Cadmium (Cd) -- Calcium (Ca) Chromium (Cr) Cobalt (Co) Copper (Cu) Iron (Fe) Lead (Pb) Lithium (Li) -- Magnesium (Mg) Manganese (Mn) Nickel (Ni) Page 3
Previous SEMI Reference # Potassium (K) Sodium (Na) N/A Tier A (Guide) Tin (Sn) -- Titanium (Ti) -- Vanadium (V) -- Zinc (Zn) 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. Page 4