1、BS EN ISO19334:2011ICS 87.040; 87.060.20NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDBinders for paintsand varnishes Gum rosin Gas-chromatographicanalysisThis British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on 31
2、March2010 BSI 2011ISBN 978 0 580 72664 6BS EN ISO 19334:2011National forewordThis British Standard is the UK implementation of EN ISO 19334:2011. It is identical to ISO 19334:2010. It supersedes BS ISO 19334:2010, which is withdrawn.The UK participation in its preparation was entrusted to TechnicalC
3、ommittee STI/3, Paints, media and related products.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application.Compliance wit
4、h a British Standard cannot confer immunityfrom legal obligations.Amendments/corrigenda issued since publicationDate Comments 30 June 2011 This corrigendum renumbers BS ISO 19334:2010 as BS EN ISO 19334:2011EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 19334 April 2011 ICS 87.040; 87.060.
5、20 English Version Binders for paints and varnishes - Gum rosin - Gas-chromatographic analysis (ISO 19334:2010) Liants pour peintures et vernis - Colophane - Analyse par chromatographie en phase gazeuse (ISO 19334:2010) Bindemittel fr Beschichtungsstoffe - Kolophonium - Gaschromatographische Analyse
6、 (ISO 19334:2010) This European Standard was approved by CEN on 17 March 2011. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bib
7、liographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the respo
8、nsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Gr
9、eece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Manage
10、ment Centre: Avenue Marnix 17, B-1000 Brussels 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 19334:2011: EBS EN ISO 19334:2011EN ISO 19334:2011 (E)ii Foreword The text of ISO 19334:2010 has been prepared by Technical Com
11、mittee ISO/TC 35 “Paints and varnishes” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 19334:2011 by Technical Committee CEN/TC 139 “Paints and varnishes” the secretariat of which is held by DIN. This European Standard shall be given the status of a nat
12、ional standard, either by publication of an identical text or by endorsement, at the latest by October 2011, and conflicting national standards shall be withdrawn at the latest by October 2011. Attention is drawn to the possibility that some of the elements of this document may be the subject of pat
13、ent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cr
14、oatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The tex
15、t of ISO 19334:2010 has been approved by CEN as a EN ISO 19334:2011 without any modification. BS EN ISO 19334:2011EN ISO 19334:2011 (E)iii iv ISO 2011 All rights reservedIntroduction Gum rosins are important commercial materials, primarily composed of rosin acids, but also containing some neutral ma
16、terial. For many applications, it is necessary to know the level of the individual rosin acids present in these products. Gas chromatography has proven to be a useful tool for such determinations (see ASTM D 509), and capillary chromatography, specified in these test methods, is considered to be the
17、 most effective gas-chromatographic technique currently available. Due to hydrogen bonding, unmodified rosin acids cannot be volatilized at atmospheric pressure without undergoing decomposition. So, it is necessary to convert the free acids to more volatile and more stable methyl esters, prior to ch
18、romatographic separation. This International Standard describes one way to prepare methyl esters. The classic method is through the use of diazomethane, but diazomethane is a hazardous and toxic material, and so is no longer the preferred agent. Trimethylphenylammonium hydroxide (TMPAH) and tetramet
19、hylammonium hydroxide (TMAH) are satisfactory methylating agents as both produce results that are very similar to those of diazomethane, but without the hazards that are associated with diazomethane. N,N-dimethylformamide dimethyl acetal (DMF-DMA) gives results comparable to those obtained with TMPA
20、H and TMAH and is easy and safe to use. However, the reagent is moisture-sensitive, requiring samples to be free of any significant levels of water. This International Standard specifies the method using TMAH. BS EN ISO 19334:2011EN ISO 19334:2011 (E)INTERNATIONAL STANDARD ISO 2011 All rights reserv
21、ed 1Binders for paints and varnishes Gum rosin Gas-chromatographic analysis 1 Scope This International Standard specifies a gas-chromatographic method for determining the amounts of certain rosin acids in gum rosin using capillary gas-chromatographic separation of the volatile methyl esters of these
22、 acids. It is intended primarily to permit the identification of gum rosin from specific species of pine trees. It is not designed for the quantitative analysis of gum rosin. If such analyses are required, the internal-standard technique specified in ASTM D 5974 should be used. 2 Normative reference
23、s The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. GB 8145, Gum rosin Test methods of rosin ASTM D
24、 509, Standard Test Methods of Sampling and Grading Rosin Naval Stores Act of 1923 (42 Stat 1435.7, USC 91-99) as amended in 1951 3 Sampling Take a representative sample following the procedures specified in GB 8145, ASTM D 509 or the Naval Stores Act of 1923 (42 Stat 1435.7, USC 91-99) as amended i
25、n 1951. NOTE Rosin samples need to be freshly broken from a larger mass to ensure the results are not affected by air oxidation of the rosin. 4 Apparatus 4.1 Gas chromatograph Use an instrument equipped with a flame-ionization detector (FID) that can be operated under the conditions given in 7.1. 4.
26、2 Column The recommended (referee) column is a fused-silica BDS column 25 m in length, 0,32 mm in internal diameter and with a 0,20 m film thickness, which gives separation equivalent to or better than that shown in Figures 1 to 3. If other columns are used, the operating conditions shall be chosen
27、such that the separation obtained is equivalent to or better than that shown in Figures 1 to 3. BS EN ISO 19334:2011EN ISO 19334:2011 (E)2 ISO 2011 All rights reserved5 Reagents and materials Reagent-grade chemicals should preferably be used in all analyses. If other grades are used, it shall be fir
28、st ascertained that the reagent concerned is of sufficiently high purity to permit its use without lessening the accuracy of the determination. 5.1 Tetramethylammonium hydroxide (TMAH) solution, 24 % in methanol, CAS No. 75-59-2 5.2 Tetramethylammonium hydroxide (TMAH) solution, 6 % in methanol. Dil
29、ute 25 ml of the reagent described in 5.1 with 75 ml of methanol. 5.3 Phenolphthalein solution, 1 % (mass per volume) in methanol 5.4 Methanol, anhydrous 5.5 Toluene (optional) 6 Preparation of methyl esters Weigh approximately 50 mg of the sample into a suitable vial, and dissolve it in 0,5 ml to 3
30、,0 ml of methanol. Add 2 to 3 drops of phenolphthalein indicator solution, and titrate to a pink colour (pH 7,8 to 8,1) with the solution of 6 % solution. When the solution is injected into the heated injection port of the chromatograph, the tetramethylammonium salts are pyrolyzed to methyl esters.
31、NOTE For solid rosin, 2 to 3 drops of toluene may be added to the vial prior to the addition of TMAH, to assist in dissolving the sample. 7 Gas-chromatographic analysis 7.1 Set-up of gas chromatograph (GC) Set the GC conditions so that they are approximately as follows (see also the last paragraph i
32、n this subclause): Column temperature: 195 C, isothermal Injection port temperature: 300 C Injection port liner: glass splitter Detector temperature: 280 C Carrier gas: hydrogen or helium Linear flow rate: 40 cm/s Split ratio: 40 to 1 Detector: FID hydrogen: 50 kPa air: 100 kPThese are the typical o
33、perating conditions for the instrument using the BDS column. The particular equipment used shall be adjusted in accordance with the manufacturers instructions to optimize its performance. Ongoing adjustment of operating temperature and flow rate may be necessary to maintain optimum performance of th
34、e column due to ageing. 7.2 Analysis Inject 0,5 l to 1,0 l of the test sample prepared in Clause 6. NOTE Dilution of the sample with additional solvent may be necessary to obtain injections that do not overload the column or detector. BS EN ISO 19334:2011EN ISO 19334:2011 (E) ISO 2011 All rights res
35、erved 37.3 Calculation Sum all the areas of the individual peaks, exclusive of the solvent peak, to obtain the total peak area. Calculate the relative percentage of each rosin acid methyl ester present, uncorrected for the amount of polymeric materials present, using the equation Tot100Rosin acid(%)
36、AA= where A is the peak area for the rosin acid methyl ester being determined; ATotis the sum of the areas of all rosin acid methyl ester peaks. NOTE See Figures 1 to 3 for typical chromatograms of selected gum rosins and Table 1 for their compositions determined from these and other such chromatogr
37、ams. 8 Test report The test report shall contain at least the following information: a) all details to identify the product tested; b) reference to this International Standard (ISO 19334:2010); c) the area percent of individual rosin acids to the nearest 0,1 %; d) by comparison with Table 1 and Figu
38、res 1 to 3, the identity of the gum rosin; e) any deviation from the test method specified; f) the date of the test. Table 1 Typical contents of characteristic rosin acids in gum rosins from pine species (determined by the gas-chromatographic method specified in this International Standard) Rosin ac
39、id Pinus massoniana Pinus merkusii Pinus elliottii Pinus pinaster Pinus caribaea Pinus keysia Pinus yunnanensis Relative Retention % % % % % % % Communic 0 0 5 0 1 0 0 0,588 Palustric 25 20 19 19 22 20 26 0,634 Isopimaric 2 15 17 5 8 4 6 0,664 Abietic 35 35 23 38 35 41 31 0,967 Dehydroabietic 4 5 5
40、6 7 4 5 1,000 Neoabietic 16 5 20 16 17 18 22 1,092 Mercusic 0 7 0 0 0 0 0 1,514 NOTE Capillary gas-liquid chromatography (GLC). Labelled peaks eluated as methyl esters. Conversion of rosin acids to their methyl deviates by means of tetramethylammonium hydroxide (TMAH) procedure. Column: fused silica
41、 BDS, l = 25 m, d = 0,32 mm, film thickness = 0,2 m, T = 195 C (isothermal), carrier gas H2at 50 kPa. BS EN ISO 19334:2011EN ISO 19334:2011 (E)4 ISO 2011 All rights reservedKey 1 palustric acid 2 isopimaric acid 3 abietic acid 4 dehydroabietic acid 5 neoabietic acid Figure 1 Chromatogram of rosin ac
42、id methyl esters from Pinus massoniana rosin BS EN ISO 19334:2011EN ISO 19334:2011 (E) ISO 2011 All rights reserved 5Key 1 palustric acid 2 isopimaric acid 3 abietic acid 4 dehydroabietic acid 5 neoabietic acid 6 mercusic acid Figure 2 Chromatogram of resin acid methyl esters from Pinus merkusii ros
43、in BS EN ISO 19334:2011EN ISO 19334:2011 (E)6 ISO 2011 All rights reservedKey 1 communic acid 2 palustric acid 3 isopimaric acid 4 abietic acid 5 dehydroabietic acid 6 neoabietic acid Figure 3 Chromatogram of resin acid methyl esters from Pinus elliotii rosin BS EN ISO 19334:2011EN ISO 19334:2011 (E
44、) ISO 2011 All rights reserved 7Bibliography 1 ASTM D 5974, Standard Test Methods for Fatty and Rosin Acids in Tall Oil Fractionation Products by Capillary Gas Chromatography BS EN ISO 19334:2011EN ISO 19334:2011 (E)ICS 87.040; 87.060.20 Price based on 7 pages ISO 2011 All rights reserved BS EN ISO
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