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SEMI C41-0301A SPECIFICATIONS AND GUIDELINES FOR 2-PROPANOL

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SEMI C41-0301A SPECIFICATIONS AND GUIDELINES FOR 2-PROPANOL C41 0301 PROPANOL
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2 PROPANOLSEMI C41 0301A SEMI 1978 20011 SEMI C41 0301A SPECIFICATIONS AND GUIDELINES FOR 2 PROPANOL These specifications and guidelines were technically approved by the Global Process Chemicals Committee and are the direct responsibility of the North American Process Chemicals Committee Current edition approved by the North American Regional Standards Committee on October 17 1999 and November 22 2000 Initially available at www semi org February 2001 to be published March 2001 This document replaces SEMI C1 15 C7 7 C8 7 and C11 7 in their entirety Originally published in 1978 1990 1992 and 1998 respectively Previously published June 1999 NOTE This document was published twice during the March 2001 0301 publishing cycle 1 Purpose 1 1 The purpose of this document is to standardize requirements for 2 propanol 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 2 propanol 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 2 propanol used in the semiconductor industry 2 2 The VLSI grade purity level is typically required by semiconductor devices with geometries of 0 8 1 2 microns 2 3 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 Standards 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 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 5 Terminology 5 1 None 6 Physical Property for information only Density at 25 C0 78 g mL Boiling Point82 3 C 7 Requirements 7 1 The requirements for 2 propanol for Grades 1 and 2 VLSI Grade and Tiers B and C are listed in Table 1 8 Grade 1 Procedures NOTE 2 Due to the uncertainty of acid concentration in the liquid residue the final concentration can be estimated to be approximately 2 v v Standard calibration solutions are to use this same acid concentration NOTE 3 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 5 micron film of DB Wax or equivalent 100 methyl silicone which has been surface bonded and cross linked Column Temperature 40 C isothermal for 5 minutes then programmed to 200 C at 10 C min Injector Temperature 150 C Detector Temperature 250 C Sample Size 0 2 L splitless Carrier Gas Helium at 3 mL min Detector Thermal Conductivity Approximate Retention Times min Acetone4 5 2 Propanol5 0 SEMI C41 0301A SEMI 1978 20012 PROPANOL2 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 a 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 phenolphthalein indicator solution Add 0 01 N sodium hydroxide until a slight pink color persists after shaking for one half minute Add 64 mL 50 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 128 mL 100 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 256 mL 200 g of sample to dryness Dry at 105 C for 30 minutes cool in a desiccator and weigh see SEMI C1 Section 3 3 Determination of Residue After Evaporation 8 6 Water Add 25 mL of methanol 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 Water H2O mL KF reagent KF factor g H2O mL 100 Weight of sample g 8 7 Solubility in Water Mix 10 mL of sample with 40 mL of water Allow to stand 1 hour The solution should be as clear as an equal volume of water 8 8 Chloride To 64 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 and dilute to 20 mL with water Add 1 mL of silver nitrate reagent solution Any turbidity produced should be no greater than that produced when 0 01 mg of chloride ion Cl is treated as the sample 8 9 Phosphate To 26 mL 20 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 25 mL of 0 5 N sulfuric acid Add 1 mL of ammonium molybdate reagent solution and 1 mL of p methylamino phenol sulfate reagent solution Allow to stand at room temperature for 2 hours Any blue color produced should be no greater than that produced when 0 01 mg of phosphate ion PO4 is treated like the sample 8 10 Arsenic and Antimony as As Evaporate 256 mL 200 g of sample in a 400 mL beaker to a small volume in a hood Add 50 mL of water and again evaporate to a small volume Repeat the evaporation with water addition Do not allow to go to dryness Add 5 mL of nitric acid and 5 mL of sulfuric acid and evaporate to dense fumes of sulfur trioxide Cool cautiously add 10 mL of water and again evaporate to dense fumes of sulfur trioxide Cool and cautiously wash into a generator flask with water to make a volume of 35 mL Proceed as described in the General Method for Arsenic and Antimony under SEMI C1 Section 3 4 5 starting with the sentence which begins Swirl the flask Any red color in the silver diethyldithiocarbamate solution of the sample should be no greater than that of the standard containing 0 002 mg of arsenic As 8 11 Trace Metal Analysis 8 11 1 Boron To 128 mL 100 g of sample add 0 10 mL of 10 sodium hydroxide and evaporate to dryness in a nitrogen atmosphere using a covered chamber such as a Thiers assembly or equivalent Dissolve the residue with 2 mL of water and 0 10 mL of hydrochloric acid Transfer to a test tube cool in an ice bath and add 10 mL of sulfuric acid Add 10 mL of carminic acid solution and remove from the ice bath Allow to stand for 45 minutes Prepare a standard containing 0 001 mg of boron treated exactly as the sample Run a complete blank determination on 2 mL of water Measure the absorbances of the sample and standard against the blank at 585 nm using 5 00 cm cells The absorbance of the sample solution should be no greater than that of the standard 8 11 1 1 Carminic Acid Solution Dissolve 0 05 g of carminic acid in 100 mL of sulfuric acid and shake until dissolution is complete 8 11 1 2 Boron Standard Solution Dissolve 0 572 g of boric acid in water in a 1000 mL volumetric flask Dilute to the mark with water Dilute 10 0 mL of this solution with water to the mark in a 100 mL volumetric flask 1 mL 0 01 mg boron 8 11 2 Gold Au Analyze by graphite atomic absorption using the manufacturer s recommended procedure This technique has been shown to give satisfactory results using a 1 4 dilution and Zeeman background correction Each laboratory must determine the appropriate dilution and background correction for their instrument to meet the specification limit 2 PROPANOLSEMI C41 0301A SEMI 1978 20013 8 11 3 The following method has given satisfactory results in determining trace metal impurities at the value specified for each of the following trace metals aluminum Al calcium Ca chromium Cr copper Cu iron Fe lead Pb magnesium Mg manganese Mn nickel Ni potassium K sodium Na tin Sn titanium Ti and zinc Zn Alternate methods may be used as long as appropriate studies demonstrate recovery between 75 125 of a known sample spike for half of the value of each specified item 8 11 4 Special Reagents 8 11 4 1 Hydrochloric Acid Ultra Pure Use hydrochloric acid specified for ultra low metal ion content 8 11 4 2 2 v v Hydrochloric Acid Solution Dilute 20 mL of ultra pure 12 M hydrochloric acid to 1 L using water meeting the criteria for Type E1 1 in ASTM D5127 8 11 5 Sample Preparation 8 11 5 1 Tin To 100 g 128 mL sample in a PTFE dish add 1 mL of 1 oxalic acid solution Slowly evaporate to about 1 mL Dissolve the residue in 10 hydrochloric acid and transfer to a 10 mL volumetric flask using 10 hydrochloric acid Analyze by plasma emission spectrometry using matrix matched standards 8 11 5 2 All Other Elements In a clean environment place 250 g of solvent in a PTFE dish Slowly evaporate on a hot plate avoiding loss of sample by effervescence or spattering until approximately 1 mL of liquid remains Take up liquid and all visible residue from walls of dish with 1 mL ultra pure 12 M hydrochloric acid and continue heating until approximately 0 5 mL of liquid remains No undissolved particulate matter should be observed Otherwise repeat the addition of hydrochloric acid until all particulate matter is dissolved Transfer quantitatively to a 50 mL volumetric flask using 2 v v hydrochloric acid and adjust liquid level to mark Prepare a reagent blank using the same reagents and in the same manner as for the sample concentration 8 11 6 Analysis 8 11 6 1 Using the prepared sample and reagent blank analyze group I elements potassium K and sodium Na by atomic absorption spectroscopy and all other elements by plasma emission spectroscopy Apply if necessary a reagent blank correction to the final determined value of the sample 9 Grade 2 Procedures NOTE 4 Each laboratory is responsible for verifying the validity of the method within its own operation 9 1 Non Metal Impurities See Section 8 which contains procedures for the following tests Assay Water Color APHA Chloride Phosphate Arsenic and Antimony as As Boron 9 2 Trace Metals Analysis 9 2 1 The following method has given satisfactory results in determining metal ion impurities at the values specified for each of the following metals aluminum Al barium Ba beryllium Be bismuth Bi calcium Ca chromium Cr cobalt Co copper Cu gallium Ga germanium Ge gold Au iron Fe lead Pb lithium Li magnesium Mg manganese Mn molybdenum Mo nickel Ni niobium Nb potassium K silver Ag sodium Na strontium Sr tantalum Ta tin Sn titanium Ti vanadium V zinc Zn and zirconium Zr Alternate methods may be used as long as appropriate studies demonstrate a recovery between 75 125 of a known sample spike for half of the value of each specified element 9 2 2 Special Reagents 9 2 2 1 Nitric Acid Ultra Pure Use nitric acid specified for low metal ion content 9 2 2 2 1 Nitric Acid Solution Dilute 10 mL of ultrapure nitric acid to 1 L using water meeting the criteria for Type E1 1 in ASTM D5127 9 2 2 3 Water The water used for all the dilution calibration and standards should meet at a minimum the criteria for Type E1 1 in ASTM D5127 in regard to cation analysis 9 2 2 4 Indium Internal Standard Make up an indium internal standard solution to a concentration of 20 mg mL ppm from an appropriate concentrated indium standard solution 9 2 2 5 Mannitol Powder Mannitol powder reagent grade ACS 9 2 2 6 5 Mannitol Solution Prepare a 5 by weight dissolve and dilute 5 g of reagent grade Mannitol powder ACS to 100 g using water meeting the criteria for Type E1 1 in ASTM D5127 SEMI C41 0301A SEMI 1978 20012 PROPANOL4 9 2 3 Sample Preparation 9 2 3 1 All Elements In a clean environment place 200 g of sample into a PTFE dish Add 5 mL of the 5 Mannitol solution and 100 mL of the 1 nitric acid solution Slowly evaporate on a hot plate to dryness avoiding loss of sample by effervescence or spattering until 1 to 2 mL remain Dissolve the residue with 5 mL of the 1 nitric acid solution by heating on a hot plate at low temperature for several minutes Cool to room temperature dilute to 50 mL with 1 nitric acid add 50 mL of the indium internal standard mix well Run a reagent blank 9 2 4 Analysis 9 2 4 1 Using the prepared solutions and blanks analyze potassium calcium and iron by graphite furnace atomic absorption GFAA and the remaining elements by inductively coupled plasma mass spectrometry ICP MS For calibration the standards are made up with the 1 nitric acid solution and a final concentration of 20 ng g of the indium internal standard 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 Grade 5 Procedures 12 1 This section does not apply to this chemical 13 VLSI Grade Procedures 13 1 Specific procedures for this grade do not exist Refer to Sections 8 and 9 for available procedures 14 Tier A Procedures 14 1 This section does not apply to this chemical 15 Tier B Procedures 15 1 Standardized test methods are being developed for all parameters at the purity levels indicated Until standardized test methods are published test method ology shall be determined by user and producer The Process Chemicals Committee considers a test method to be valid only if there is a documented recovery study showing a recovery of 75 125 Recovery is for a known sample spike at 50 of the specified level 16 Tier C Procedures 16 1 Standardized test methods are being developed for all parameters at the purity levels indicated The Process Chemicals Committee considers a test method to be valid if there is a documented recovery study showing a recovery of 75 125 Recovery is for a known sample spike at 50 of the specified level 17 Tier D Procedures 17 1 This section does not apply to this chemical Table 1 Impurity Limits and Other Requirements for 2 Propanol Previous SEMI Reference C1 15 96C7 7 93C11 7 0698C8 7 92 Grade 1Grade 2VLSI GradeTier BTier C Specification Specification Guideline Guideline Guideline Assay CH3CHOHCH3 99 5 min99 8 min 98 8 min99 8 min Assay gc 99 7 min Color APHA 10 max10 max10 max10 max10 max Residue after Evaporation5 ppm max5000 ppb max5 ppm max500 ppb max1 ppm max Resistivity 15 MegOhm cm min Solubility in WaterTo pass test Chloride Cl 0 2 ppm max200 ppb max0 2 ppm max50 ppb max50 ppb max Nitrate NO3 50 ppb max50 ppb max Phosphate PO4 0 5
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