BS EN ISO 19334-2011 Binders for paints and varnishes Gum rosin Gas-chromatographic analysis《色漆和清漆用粘合剂 脂松香 气相色谱分析》.pdf

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-chromatographicanalysisLicensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/10/2011 03:31, Uncontrolled Copy, (c) BSIThis B

2、ritish Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee on 31 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

3、 19334:2010, which is withdrawn.The UK participation in its preparation was entrusted to TechnicalCommittee STI/3, Paints, media and related products.A list of organizations represented on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

4、necessary provisionsof a contract. Users are responsible for its correct application.Compliance with 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 1933

5、4:2011Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/10/2011 03:31, Uncontrolled Copy, (c) BSIEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 19334 April 2011 ICS 87.040; 87.060.20 English Version Binders for paints and varnishes - Gum rosin - Gas-chromatographic analysis (ISO 19

6、334:2010) Liants pour peintures et vernis - Colophane - Analyse par chromatographie en phase gazeuse (ISO 19334:2010) Bindemittel fr Beschichtungsstoffe - Kolophonium - Gaschromatographische Analyse (ISO 19334:2010) This European Standard was approved by CEN on 17 March 2011. CEN members are bound t

7、o 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 bibliographical references concerning such national standards may be obtained on application to the CEN-C

8、ENELEC 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 responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has

9、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, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Pol

10、and, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2011 CEN All rights of exploitation in any form and by

11、any means reserved worldwide for CEN national Members. Ref. No. EN ISO 19334:2011: ELicensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/10/2011 03:31, Uncontrolled Copy, (c) BSIBS EN ISO 19334:2011EN ISO 19334:2011 (E)ii Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/10/2011 03:31,

12、Uncontrolled Copy, (c) BSIForeword The text of ISO 19334:2010 has been prepared by Technical Committee 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” th

13、e secretariat of which is held by DIN. This European Standard shall be given the status of a national 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

14、is drawn to the possibility that some of the elements of this document may be the subject of patent 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 f

15、ollowing countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, S

16、lovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text 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 Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/10/2011

17、 03:31, Uncontrolled Copy, (c) BSIiv ISO 2011 All rights reservedIntroduction Gum rosins are important commercial materials, primarily composed of rosin acids, but also containing some neutral material. For many applications, it is necessary to know the level of the individual rosin acids present in

18、 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 most effective gas-chromatographic technique currently available. Due to hydrogen bonding, unmodified ro

19、sin 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 chromatographic separation. This International Standard describes one way to prepare methyl esters. The cla

20、ssic 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 tetramethylammonium hydroxide (TMAH) are satisfactory methylating agents as both produce results that are very si

21、milar 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 TMPAH and TMAH and is easy and safe to use. However, the reagent is moisture-sensitive, requiring samples to

22、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)Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/10/2011 03:31, Uncontrolled Copy, (c) BSIINTERNATIONAL STANDARD ISO 2011 All rights reserved 1Bi

23、nders 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 acids

24、. 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 references The

25、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 509,

26、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 in 1951

27、. 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. 4.2 Colu

28、mn 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 such t

29、hat 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)Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/10/2011 03:31, Uncontrolled Copy, (c) BSI2 ISO 2011 All rights reserved5 Reagents and materials Reagent-grade c

30、hemicals should preferably be used in all analyses. If other grades are used, it shall be first 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 meth

31、anol, CAS No. 75-59-2 5.2 Tetramethylammonium hydroxide (TMAH) solution, 6 % in methanol. Dilute 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

32、 Weigh approximately 50 mg of the sample into a suitable vial, and dissolve it in 0,5 ml to 3,0 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 inject

33、ion port of the chromatograph, the tetramethylammonium salts are pyrolyzed to methyl esters. 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) S

34、et the GC conditions so that they are approximately as follows (see also the last paragraph in 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: 4

35、0 cm/s Split ratio: 40 to 1 Detector: FID hydrogen: 50 kPa air: 100 kPThese are the typical operating 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

36、of operating temperature and flow rate may be necessary to maintain optimum performance of the 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 overl

37、oad the column or detector. BS EN ISO 19334:2011EN ISO 19334:2011 (E)Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/10/2011 03:31, Uncontrolled Copy, (c) BSI ISO 2011 All rights reserved 37.3 Calculation Sum all the areas of the individual peaks, exclusive of the solvent peak, to obtain t

38、he 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(%)AA= where A is the peak area for the rosin acid methyl ester being determined; ATotis the sum of the areas o

39、f 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 chromatograms. 8 Test report The test report shall contain at least the following information: a) all details to ident

40、ify 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 Figures 1 to 3, the identity of the gum rosin; e) any deviation from the test method specified; f) the date of t

41、he 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 acid Pinus massoniana Pinus merkusii Pinus elliottii Pinus pinaster Pinus caribaea Pinus keysia Pinus yunnanen

42、sis 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 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 ch

43、romatography (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 BDS, l = 25 m, d = 0,32 mm, film thickness = 0,2 m, T = 195 C (isothermal), carrier gas H2at 50 kPa. BS EN

44、ISO 19334:2011EN ISO 19334:2011 (E)Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/10/2011 03:31, Uncontrolled Copy, (c) BSI4 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 acid methyl

45、 esters from Pinus massoniana rosin BS EN ISO 19334:2011EN ISO 19334:2011 (E)Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/10/2011 03:31, Uncontrolled Copy, (c) BSI ISO 2011 All rights reserved 5Key 1 palustric acid 2 isopimaric acid 3 abietic acid 4 dehydroabietic acid 5 neoabietic acid

46、 6 mercusic acid Figure 2 Chromatogram of resin acid methyl esters from Pinus merkusii rosin BS EN ISO 19334:2011EN ISO 19334:2011 (E)Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/10/2011 03:31, Uncontrolled Copy, (c) BSI6 ISO 2011 All rights reservedKey 1 communic acid 2 palustric acid

47、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)Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/10/2011 03:31, Uncontrolled Copy, (c) BSI ISO 2011 A

48、ll 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)Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/10/2011 03:31, Uncontrolled Copy, (c)

49、BSIICS 87.040; 87.060.20 Price based on 7 pages ISO 2011 All rights reserved BS EN ISO 19334:2011EN ISO 19334:2011 (E)Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/10/2011 03:31, Uncontrolled Copy, (c) BSIThis page has been intentionally left blankLicensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 10/10/2011 03:31, Uncontrolled Copy, (c) BSIBSI GroupHeadquarters 389Chiswick High Road,London, W4 4AL, UKTel +44 (0)20 8996 9001Fax +44 (0)20 8996 - British Standards Institut