SEMI C19-0301 SPECIFICATION FOR ACETONE.pdf.pdf

ACETONESEMI C19-0301 SEMI 1978, 20011 SEMI C19-0301 SPECIFICATION FOR ACETONE This specification was technically approved by the Global Process Chemicals Committee and is the direct responsibility of the North American Process Chemicals Committee. Current edition approved by the North American Regional Standards Committee on October 17, 1999. Initially available at www.semi.org February 2001; to be published March 2001. This document replaces SEMI C1.2 in its entirety. Originally published in 1978; previously published June 1999. 1 Purpose 1.1 The purpose of this document is to standardize requirements for acetone used in the semiconductor industry and testing procedures to support those standards. Test methods have been shown to give statistically valid results. This document also provides guidelines for grades of acetone for which a need has been identified. In the case of the guidelines, the test methods may not have been statistically validated yet. 2 Scope 2.1 The scope of this document is all grades of acetone used in the semiconductor industry. 2.2 These standards do not purport to address safety issues, if any, associated with their use. It is the responsibility of the user of these standards to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 3 Limitations 3.1 None. 4 Referenced Documents 4.1 SEMI Standards SEMI C1 Specifications for Reagents 4.2 ASTM Standards1 ASTM D5127 Standard Guide for Ultra Pure Water Used in the Electronics and Semiconductor Industry NOTE 1: As listed or revised, all documents cited shall be the latest publications of adopted standards. 5 Terminology 5.1 None. 6 Physical Property (for information only) Density at 25C0.79 g/mL Boiling Point56.3C 1 American Society for Testing and Materials, 100 Barr Harbor Drive, West Conshohocken, Pennsylvania 19428-2959, USA. Telephone: 610.832.9585, Fax: 610.832.9555. Website: www.astm.org 7 Requirements 7.1 The requirements for acetone for Grade 1 are listed in Table 1. 8 Grade 1 Procedures NOTE 2: Each laboratory is responsible for verifying the validity of the method within its own operation. 8.1 Assay Analyze the sample by gas chromatography (see SEMI C1, Section 3.1, Guidelines for Assay by Wide Bore Column Gas Chromatography). The parameters cited have given satisfactory results. Column: 30 meter 530 micron I.D.-fused silica capillary, coated with 1 mm film of DB-1701 or equivalent (14% cyanopropyphenyl which has been surface bonded and crosslinked). Column Temperature: 40C isothermal for 5 minutes, then programmed to 200C at 10C/min. Injector Temperature:150C Detector Temperature:250C Sample Size:1 L split Carrier Gas:Helium at 3 mL/min Detector:Flame Ionization Approximate Retention Times (min): Methanol1.1 Acetaldehyde2.3 Acetone2.9 Isopropanol3.3 Cumene10.0 Mesityl Oxide11.8 Diacetone Alcohol12.0 8.2 Color Dilute 2.0 mL of platinum-cobalt stock solution (APHA No. 500) to 100 mL with water. Compare this standard (APHA No. 10) with 100 mL of sample in Nessler tubes. View vertically over white background. The sample must be no darker than the standard. 8.3 Acidity To 25 mL of water in a glass-stoppered flask, add 10 mL of sample and 0.1 mL of SEMI C19-0301 SEMI 1978, 2001ACETONE2 phenolphthalein indicator solution. Add 0.01 N sodium hydroxide until a slight, pink color persists after shaking for one-half minute. Add 42 mL (33 g) of the sample, mix well, and titrate with 0.01 N sodium hydroxide until the pink color is reproduced. Not more than 1.0 mL of the sodium hydroxide solution should be required. 8.4 Alkalinity Add 25 mL (20 g) of sample to 25 mL of water and mix well. Add 0.05 mL of methyl red indicator solution. Titrate with 0.01 N hydrochloric acid until a slight pink color is produced. Not more than 1.0 mL of the hydrochloric acid should be required. 8.5 Residue after Evaporation Evaporate 253 mL (200 g) of sample to dryness. Dry at 105C for 30 min- utes, cool in a desiccator, and weigh (see SEMI C1, Section 3.3, Determination of Residue After Evaporation). 8.6 Water Add 25 mL of pyridine to a dry titration flask and add Karl Fischer (KF) reagent to a visually or electrometrically determined endpoint that persists for 30 seconds. Add 25 mL (20 g) of sample, taking care to protect the sample and contents of the flask from moisture. Stir vigorously and titrate with Karl Fischer reagent to the same endpoint. % WaterH 2O () = mL KF reagent KF factorg H2O mL()100 Weight of sampleg( ) 8.7 Solubility in Water Mix 40 mL of sample with 40 mL of water. Allow to stand for 30 minutes. The solution should be as clear as an equal volume of water. 8.8 Chloride To 63 mL (50 g) of sample, add 10 mL of sodium carbonate reagent solution and evaporate to dryness on a steam bath in a hood. Dissolve the residue in 10 mL of water. Add 1 mL of nitric acid, dilute to 20 mL with water, and add 1 mL of silver nitrate reagent solution. Any turbidity produced should be no greater