ASTM D3156-1996(2005) Standard Practice for Rubber&8212 Chromatographic Analysis of Antidegradants (Antioxidants Antiozonants and Stabilizers)《橡胶的标准实施规程 防降解剂(防氧化剂、防臭氧剂及稳定剂)的色谱分析》.pdf
《ASTM D3156-1996(2005) Standard Practice for Rubber&8212 Chromatographic Analysis of Antidegradants (Antioxidants Antiozonants and Stabilizers)《橡胶的标准实施规程 防降解剂(防氧化剂、防臭氧剂及稳定剂)的色谱分析》.pdf》由会员分享,可在线阅读,更多相关《ASTM D3156-1996(2005) Standard Practice for Rubber&8212 Chromatographic Analysis of Antidegradants (Antioxidants Antiozonants and Stabilizers)《橡胶的标准实施规程 防降解剂(防氧化剂、防臭氧剂及稳定剂)的色谱分析》.pdf(5页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: D 3156 96 (Reapproved 2005)Standard Practice forRubberChromatographic Analysis of Antidegradants(Antioxidants, Antiozonants and Stabilizers)1This standard is issued under the fixed designation D 3156; the number immediately following the designation indicates the year oforiginal adoptio
2、n or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice covers the detection and identification bythin-layer chromat
3、ography of antidegradants (antioxidants,antiozonants, and stabilizers) that may be present in raw rubberor rubber products. Analysis for other types of antidegradantsis possible as long as the requirements of the practice are met.1.2 The values stated in SI units are to be regarded as thestandard.1.
4、3 This standard does not purport to address all of thesafety concerns, if any, associated with its 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.2. Referenced Doc
5、ument2.1 ASTM Standards:2D 297 Test Methods for Rubber ProductsChemicalAnalysis3. Summary of Practice3.1 A simplified procedure (Method A, Section 13.1) basedon a single-solvent system is presented, which provides for theidentification of known materials. This may be used to checkthe presence or abs
6、ence in a rubber vulcanizate or raw rubber,of an antidegradant which should be present. However, sincethe chromatograms obtained may not be absolutely specific forany given antidegradant, a more detailed scheme is given in13.2.3.2 Method B, Section 13.2, using additional solvents andsprays is includ
7、ed, which enables a greater degree of separationof the spots to be made and therefore may enable detection andidentification of an unknown antidegradant.3.3 Other techniques, for example: gas chromatographic(with or without treatment to obtain derivatives), spectroscopic(ultraviolet and infrared), m
8、ore sophisticated thin-layer varia-tions (two dimensional techniques), may be applied to identi-fication of spots for improved detection and identification of anunknown antidegradant.3.4 It is possible that the chromatographic pattern of oneantidegradant may overlap that of another antidegradant;the
9、refore each laboratory must prepare its own referencestandards, based on the technique chosen from this practice.4. Significance and Use4.1 This practice is useful for the examination of rubbercompounds or products for the presence of chemicals thatprevent or greatly reduce degradation due to oxygen
10、, ozone, orother agents.4.2 This practice is suitable for quality assurance, factorycontrol, and research and development applications.5. Interferences5.1 In the absence of extender oils, antidegradants areextracted from the rubber by a solvent and the evaporatedextract is applied directly to a thin
11、-layer chromatographicplate.5.2 In the presence of extender oils, the oils are removed byeither a pre-treatment of the plate, with light petroleum ether orby a column chromatographic technique.5.3 Identification of the antidegradant is made by thestandard technique of thin-layer chromatography, here
12、in de-scribed.6. Apparatus6.1 Spreading Device, for making thin layer chromato-graphic plates with a coating 250 to 300 m thick.6.2 Glass Plates, 200 by 200-mm, or suitable for theselected tank. As an alternative to preparing plates, the use ofprecoated plates with a coating of 250 to 300 m is permi
13、tted.Precoated film-backed plates are not recommended.6.3 Drying Oven, 105C minimum.6.4 Desiccator, or drying box for storing plates at fixedhumidity.1This practice is under the jurisdiction of ASTM Committee D11 on Rubber andis the direct responsibility of Subcommittee D11.11 on Chemical Analysis.C
14、urrent edition approved Dec. 1, 2005. Published February 2006. Originallyapproved in 1973. Last previous edition approved in 2001 as D 3156 96 (2001).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStand
15、ards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.5 Micro-pipets, 5 and 10-mm3(L).6.6 Chromatographic Developing Tank, of a size suitable tohold
16、 plates, approximately 250 by 250 by 70 mm to 330 by 240by 110 mm. Small “sandwich-type” tanks are not recom-mended. Add about 200 cm3of developing solvent (7.4)tothetank, swirl, cover, and allow to stand 15 min before using. Tankmay be reused by repeating the swirling and standing step, aslong as t
17、he solvent ratio remains constant.6.7 Extraction Apparatus, in accordance with Section 18 or25 of Test Methods D 297.6.8 Chromatographic Columns, short, liquid-solid. Thosefound satisfactory are as follows:6.8.1 Hypodermic Syringe Barrel, 5-cm3, fitted with aneedle about 35 mm in length and 1.27 mm
18、outside diameter(No. 18 BWG).6.8.2 Glass Tubes, 120 mm in length and 10 to 12 mm indiameter, holding about 5 cm3of silica gel.7. Reagents7.1 Plate AdsorbentSilica gel containing calcium sulfate.3Silica gel containing a fluorescent indicator may be useful insome cases to allow visualization of spots
19、(before spraying)with ultraviolet light.7.2 Column AdsorbentSilica gel 200 to 600 m (30 to70-mesh),3activated by drying at 110C for at least 2 h, if dryin that period, or overnight (616 h) for convenience.7.3 SolventsUse of fume hoods with volatile and toxicsolvents is mandatory. Approved health and
20、 safety precautionsshould be observed for the use of any solvent or chemicalmentioned in this procedure. ACS grade or equivalent shouldbe used.7.3.1 Methanol.7.3.2 Acetone.7.3.3 Isopropanol.7.3.4 Light Petroleum Ether.7.3.5 Chloroform.7.3.6 Toluene.7.3.7 Ethyl Acetate.7.3.8 n-Hexane.7.3.9 n-Heptane.
21、7.3.10 Cyclohexane.7.3.11 Diethylamine.7.3.12 Ammonium Hydroxide (NH4OH, 2830 % ammoniaNH3).7.3.13 WaterReferences to water shall be understood tomean distilled water or water of equal purity.7.4 Developing Solvents:7.4.1 Test Method A90 parts n-heptane and 10 parts ethylacetate by volume.7.4.2 Test
22、 Method B, used in the following order:7.4.2.1 Toluene.7.4.2.2 95 parts toluene and 5 parts ethyl acetate by volume.7.4.2.3 75 parts cyclohexane and 25 parts diethylamine byvolume.7.4.2.4 50 parts toluene and 50 parts n-heptane by volume.7.4.3 Additional developing solvents which may proveuseful for
23、 special problems:7.4.3.1 100 parts toluene, 5 parts acetone and 0.1 partammonium hydroxide (NH4OH).7.4.3.2 100 parts toluene, 5 to 10 parts acetone and 0.1 to0.2 parts NH4OH.7.5 Spray Reagents for Color Development:7.5.1 Amines:7.5.1.1 Diazotized Sulfanilic Acid0.5 g of sulfanilic acidand 0.5 g of
24、potassium nitrite (KNO2) dissolved in 100 cm3of1 M hydrochloric acid (HCl). Make fresh daily.7.5.1.2 Benzoyl Peroxide (4 % solution in toluene).7.5.1.3 Tollens Reagent (0.5 cm3of 5 % silver nitrate(AgNO3) solution + 2 drops of 2 M sodium hydroxide (NaOH).Dissolve the precipitate in as little 2 % amm
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