ASTM D3329-2003 Standard Test Method for Purity of Methyl Isobutyl Ketone by Gas Chromatography《气相色谱法测定甲基异丁基酮纯度的标准试验方法》.pdf
《ASTM D3329-2003 Standard Test Method for Purity of Methyl Isobutyl Ketone by Gas Chromatography《气相色谱法测定甲基异丁基酮纯度的标准试验方法》.pdf》由会员分享,可在线阅读,更多相关《ASTM D3329-2003 Standard Test Method for Purity of Methyl Isobutyl Ketone by Gas Chromatography《气相色谱法测定甲基异丁基酮纯度的标准试验方法》.pdf(4页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: D 3329 03Standard Test Method forPurity of Methyl Isobutyl Ketone by Gas Chromatography1, 2This standard is issued under the fixed designation D 3329; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last re
2、vision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope*1.1 This test method covers the determination
3、of the purityof methyl isobutyl ketone (MIBK) by gas chromatography andin addition provides a means for measuring certain impuritiessuch as methyl isobutyl carbinol which are of interest. Impu-rities such as water and acidity are measured by other appro-priate ASTM procedures and the results are use
4、d to normalizethe chromatographic value.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 The following applies to all specified limits in thisstandard; for purposes of determining conformance with thisstandard, an observ
5、ed value or a calculated value shall berounded off “to the nearest unit” in the last right-hand digitused in expressing the specification limit, in accordance withthe round-off method of Practice E 29.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with it
6、s use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.1.5 For specific hazard information and guidance, see thesuppliers Material Safety Data Sheet for the materials li
7、sted inthis test method.2. Referenced Documents2.1 ASTM Standards:2D 1364 Test Method for Water in Volatile Solvents (KarlFischer Reagent Titration Method)D 1613 Test Method for Acidity in Volatile Solvents andChemical Intermediates Used in Paint, Varnish, Lacquer,and Related ProductsD 2593 Test Met
8、hod for Butadiene Purity and HydrocarbonImpurities by Gas ChromatographyE 180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty ChemicalsE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE 260 P
9、ractice for Packed Column Gas Chromatography3. Summary of Test Method3.1 A representative specimen is introduced onto a gas-liquid partition column. Methyl isobutyl ketone is separatedfrom impurities such as acetone, 2-propanol, pentanone, mesi-tyl oxide, methyl isobutyl carbinol, and several uniden
10、tifiedcompounds as the components are transported through thecolumn by an inert carrier gas. The separated components aremeasured in the effluent by a detector and recorded as achromatogram. The chromatogram is interpreted by applyingcomponent attenuation and detector response factors to thepeak are
11、as, and the relative concentrations are determined byrelating the individual peak responses to the total peak re-sponse. Water and acidity are measured in accordance with TestMethods D 1364 and D 1613 and the results are used tonormalize the values obtained by gas chromatography.4. Significance and
12、Use4.1 This test method provides a measurement of commonlyfound impurities in commercially available methyl isobutylketone. The measurement of these impurities and the resultsthereof can individually or when totaled and subtracted from100 (assay) be used for specification acceptance.5. Apparatus5.1
13、ChromatographAny gas liquid chromatographic in-strument having either a thermal conductivity or flame ioniza-tion detector provided the system has sufficient sensitivity andstability to obtain for 0.01 % of impurity a recorder deflectionof at least 2 mm at a signal-to-noise ratio of at least 5 to 1.
14、 Thespecimen size used in judging the sensitivity must be such thatthe column is not overloaded, which would result in peak1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.3
15、5 on Solvents, Plasticizers, and Chemical Intermediates.Current edition approved Dec.1, 2003. Published December 2003. Originallyapproved in 1974. Last previous edition approved in 1999 as D 3329 99.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service
16、 at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2
17、959, United States.broadening, loss of resolution, shifting retention times andformation of leading peaks.5.2 ColumnAny column capable of resolving methylisobutyl ketone from the impurities that may be present.Possible impurities are hydrocarbons, acetone, 2-propanol,2-pentanone, 3-pentanone, mesity
18、l oxide, mesityl oxide iso-mer, and methyl isobutyl carbinol. Columns that meet thisrequirement are described in Table 1. Other columns, includingcapillary columns, may be used, provided the user establishesthat a column gives the required separation and the peak shapesare satisfactory for measureme
19、nt so that the precision require-ments of Section 12 are met.5.3 Specimen Introduction SystemAny system capable ofintroducing a representative specimen onto the column. Mi-crolitre syringes have been used successfully.5.4 RecorderA recording potentiometer with a full-scaledeflection of 5 mV or less,
20、 full-scale response time of2sorless, and sufficient sensitivity and stability to meet the require-ments of 5.1.6. Reagents and Materials6.1 Carrier GasCarrier gas appropriate to the type ofdetector used. Helium or hydrogen may be employed withthermal conductivity detectors and nitrogen, helium, or
21、argonwith flame ionization detectors. The minimum purity of thecarrier gas used should be 99.95 mol %. (WarningIf hydro-gen is used, take special safety precautions to ensure that thesystem is free from leaks and that the effluent is ventedproperly.)6.2 Column Materials:6.2.1 Liquid PhaseThe materia
22、ls successfully used incooperative test work are listed in Table 1. (See Note 1.)NOTE 1Suppliers of liquid phases and supports can be found inResearch Report RR:D01-1042, available from ASTM InternationalHeadquarters.6.2.2 Solid SupportThe materials and their mesh sizessuccessfully used in cooperati
23、ve work are shown in Table 1.(See Note 1.)6.2.3 Tubing MaterialCopper, stainless steel, and alumi-num have been found satisfactory for column tubing. Thetubing must be nonreactive with the substrate, sample, andcarrier gas and be of uniform internal diameter.6.3 Standards for Calibration and Identif
24、icationStandardsamples of all components present are needed for identificationby retention time and for calibration for quantitative measure-ments.7. Preparation of Apparatus7.1 Column PreparationThe method used to prepare thecolumn is not critical provided that the finished columnproduces the requi
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