इंटरनेट मानक Disclosure to Promote the Right To Information Whereas the Parliament of India has set out to provide a practical regime of right to information for citizens to secure access to information under the control of public authorities, in order to promote transparency and accountability in the working of every public authority, and whereas the attached publication of the Bureau of Indian Standards is of particular interest to the public, particularly disadvantaged communities and those engaged in the pursuit of education and knowledge, the attached public safety standard is made available to promote the timely dissemination of this information in an accurate manner to the public. “जान1 का अ+धकार, जी1 का अ+धकार” “प0रा1 को छोड न’ 5 तरफ” Mazdoor Kisan Shakti Sangathan Jawaharlal Nehru “The Right to Information, The Right to Live” “Step Out From the Old to the New” IS 16042-1 (2012): Cigarettes - Determination of Water in Smoke Condensates, Part 1: Gas-Chromatographic Method [FAD 4: Tobacco and Tobacco Products] “!ान $ एक न’ भारत का +नम-ण” Satyanarayan Gangaram Pitroda ““IInnvveenntt aa NNeeww IInnddiiaa UUssiinngg KKnnoowwlleeddggee”” “!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता हहहहै””ै” Bhartṛhari—Nītiśatakam “Knowledge is such a treasure which cannot be stolen” IS 16042 (Part 1) : 2012 ISO 10362-1 : 1999 Hkkjrh; ekud flxjsV èkwez la?kfur inkFkZ esa ty Kkr djuk — Hkkx 1 xSl&ØksesVksxzkfiQd i¼fr Indian Standard CIGARETTES — DETERMINATION OF WATER IN SMOKE CONDENSATES PART 1 GAS-CHROMATOGRAPHIC METHOD ICS 65.160 © BIS 2012 B U R E A U O F I N D I A N S T A N D A R D S MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG NEW DELHI 110002 December 2012 Price Group 4 Tobacco and Tobacco Products Sectional Committee, FAD 4 NATIONAL FOREWORD This Indian Standard (Part 1) which is identical with ISO 10362-1 : 1999 ‘Cigarettes — Determination of water in smoke condensates — Part 1: Gas-chromatographic method’ issued by the International Organization for Standardization (ISO) was adopted by the Bureau of Indian Standards on the recommendation of the Tobacco and Tobacco Products Sectional Committee and approval of the Food and Agriculture Division Council. The text of ISO Standard has been approved as suitable for publication as an Indian Standard without deviations. Certain conventions are, however, not identical to those used in Indian Standards. Attention is particularly drawn to the following: a) Wherever the words ‘International Standard’ appear referring to this standard, they should be read as ‘Indian Standard’. b) Comma (,) has been used as a decimal marker while in Indian Standards, the current practice is to use a point (.) as the decimal marker. In this adopted standard, reference appear to the following International Standard for which Indian Standard also exists. The corresponding Indian Standard which is to be substituted in its place is listed below along with its degree of equivalence for the edition indicated: International Standard Corresponding Indian Standard Degree of Equivalence ISO 4387 : 2000 Cigarettes — IS 16023 : 2012 Cigarettes — Identical Determination of total and nicotine-free Determination of total and nicotine- dry particulate matter using a routine free dry particulate matter using a analytical smoking machine routine analytical smoking machine For the purpose of deciding whether a particular requirement of this standard is complied with, the final value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in accordance with IS 2 : 1960 ‘Rules for rounding off numerical values (revised)’. The number of significant places retained in the rounded off value should be the same as that of the specified value in this standard. IS 16042 (Part 1) : 2012 ISO 10362-1 : 1999 Indian Standard CIGARETTES — DETERMINATION OF WATER IN SMOKE CONDENSATES PART 1 GAS-CHROMATOGRAPHIC METHOD 1 Scope This part of ISO10362 specifies a method for the gas-chromatographic determination of water in cigarette smoke condensates. The smoking of cigarettes and collection of mainstream smoke are normally carried out in accordance with ISO4387. However, the method of this part of ISO10362 is applicable to the determination of water in smoke condensatesobtainedbynon-standardsmoking. NOTE In countries not in a position to use the gas-chromatographic method, the determination of water in smoke condensatesshouldbeperformedbyaKarlFischermethod(ISO10362-2).Insuch cases, valuesobtained forwater insmoke condensatemaybeusedwiththeadditionofanotemadeintheexpressionoftheresults. 2 Normative reference The following normative document contains provisions which, through reference in this text, constitute provisions of this part of ISO10362. For dated references, subsequent amendments to, or revisions of, this publication do not apply. However, parties to agreements based on this part of ISO10362 are encouraged to investigate the possibility of applying the most recent edition of the normative document indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid InternationalStandards. ISO4387, Cigarettes—Determinationoftotalandnicotine-freedryparticulatematterusingaroutineanalytical smokingmachine. 3 Principle The smoke condensate from the mainstream smoke is dissolved in a solvent containing an internal standard. The watercontentofanaliquotofthesolutionisdeterminedbygaschromatography,andthewatercontentofthewholeof thesmokecondensateiscalculated. 4 Reagents Useonlyreagentsofrecognizedanalyticalreagentgrade. 4.1 Carriergas:heliumornitrogen(seenotein6.2). 4.2 Propan-2-ol,withmaximumwatercontentof1,0mg/ml. 4.3 Internalstandard:ethanol,ormethanol(ofpurityatleast99%). 4.4 Extraction solvent: propan-2-ol (4.2) conta ining an appropriate concentration of internal standard (4.3), normally5ml/l. 1 IS 16042 (Part 1) : 2012 ISO 10362-1 : 1999 Solventnotstoredinatemperature-controlledlaboratoryshallbeallowedtoequilibrateto(22(cid:2)2)(cid:3)Cbeforeuse. 4.5 Referencesubstance:distilledwaterordeionizedwater. 4.6 Calibrationsolutions Prepareaseries of at leastfour calibration solutions whoseconcentrations of addedwater cover the rangeexpected to be found in the test portion (usuallyup to 4mg/ml) byadding weighed amounts of water (4.5) to the solvent (4.4). Oneofthesecalibrationsolutionsshallbethesolventwithnoaddedwater(solventblank). Topreventwater beingabsorbed,thebulk solventcontainer shallbefittedwitha water trapandallsolutionsshallbe kept sealed. The solvent shall be stirred continuously to ensure the homogeneity of the water concentration in the solvent.Thecalibrationsolutionsshallbemadeupusinganextractionsolventfromthesamebatchusedin6.1. Itisrecommendedthatthecalibrationsolutionsbemadeupatleasteachweek. 5 Apparatus Usuallaboratoryapparatusand,inparticular,thefollowingitems. 5.1 Gas-chromatograph, equipped with a thermal conductivity detector, recorder and integrator or other suitabledata-handlingequipment. Glasswareandseptaforvialsshouldbestoredinadesiccatoruntiluse. 5.2 Column,ofinternaldiameterbetween2mmand4mmandpreferablyoflength1,5mto2m. Stationaryphase:PorapakQ1) 150(cid:4)m (100mesh)to190(cid:4)m (80mesh). The column is preferably made of deactivated stainless steel but other materials such as glass or nickel may be used.Alternativestationaryphases,suchasPorapak QS1)orChromosorb1021),maybeused. 5.3 Dispensingsystem,preferablyautomated,capableofdeliveringtherequiredvolumeofsolvent(4.4). Thedispensingsystem shouldbeflushedpriortousebydispensingavolumeofsolventof at least50ml which will thenberejected. 6 Procedure 6.1 Test portion Preparethetestportionbydissolvingthesmokecondensateobtainedbythemachinesmokingofaknownnumberof cigarettes in a fixed volumeof the solvent(4.4) of 20ml for 44mm discs or 50ml for 92mm discs, ensuring that the disc is fully covered. The volume may be adjusted to give a concentration of water appropriate for the calibration graph (see 6.3) provided that there is an adequate volume for effective extraction of the smoke condensate. For standardsmoking,seeISO4387. 1) PorapakQ,PorapakQSandChromosorb102aretradenamesofexamplesofsuitableproductsavailablecommercially.This informationisgivenfortheconvenienceofusersofthispartofISO10362anddoesnotconstituteanendorsementbyISOofthese products. 2 IS 16042 (Part 1) : 2012 ISO 10362-1 : 1999 6.2 Settingupthe apparatus Set up the apparatus and operate the gas chromatograph (5.1) in accordance with the manufacturer's instructions. Ensure that the peaks for water, the internal standard and solvent are well resolved, the analysis time being about 4min.Conditionthesystemjustpriortousebyinjectinga2(cid:4)laliquotoftheextractionsolventasaprimer. Suitableoperatingconditionsareasfollows: (cid:1) columntemperature:170(cid:3)C(isothermal); (cid:1) injectiontemperature:250(cid:3)C; (cid:1) detectortemperature:250(cid:3)C; (cid:1) carriergas:heliumataflowrateofabout30ml/min; (cid:1) injectionvolume:2µl. NOTE Nitrogenmayalsobeusedasanalternativecarriergasifthedetectorsensitivityissufficientlyhigh. 6.3 Calibrationof thegas chromatograph Injectanaliquot(2(cid:4)l)ofeachofthecalibrationsolutions(4.6)intothegaschromatograph.Recordthepeakareas(or heights)ofthewaterandinternalstandard(4.3).Carryoutthedeterminationatleasttwice. Calculatetheratioofthewaterpeak totheinternalstandardpeak from thepeak area(or height) datafor eachof the calibration solutions including the solvent blank. Plot the graph of the concentrations of added water in accordance withthearearatiosorcalculatealinearregressionequationfromthesedata.Usethelinearregressionequation. Perform this full calibration procedure daily. In addition, inject an aliquot of an intermediate concentration standard after every 20 sample determinations. If the calculated concentration for this solution differs by more than 5% from theoriginalvalue,repeatthefullcalibrationprocedure. NOTE Theregressionlinedoesnotpassthroughzeroduetowaterpresentintheextractionsolvent. Ifthewatercontentofthesolventexceeds1,0mg/ml,thebatchshouldberejected. 6.4 Blank test Duetotheabsorptionofwaterbysmoketrapsandsolvent,itisnecessarytodetermineavalueforthesampleblank. Preparesampleblanksbytreatingadditionalsmoketrapsincludingfilters(atleast2per100cigarettessmoked)inthe same manner as that used for smoke collection. Place them near the smoking machine during smoking and extract andanalysethemtogetherwiththesmokesamples. 6.5 Determination Injectaliquots(2µl)ofthetestportionfromthesmoketraps(see6.1)andblank traps(see6.4).Calculatetheratioof thewaterpeak/internalstandardpeakfromthepeakarea(orheight)data. Carry out the determination at least twice under identical conditions. Calculate the mean value of the ratio from the replicatedeterminations. NOTE Where results are obtained from a number of separate channels of smoking and where an autosampler is used, a singlealiquotportionfromthesmoketrapsisconsideredadequate. 3 IS 16042 (Part 1) : 2012 ISO 10362-1 : 1999 7 Expression of results Calculate the water concentration of the smoke trap and blank trap extracts using the graph or linear regression equationpreparedin6.3. Thewatercontentofthesmoke,m ,inmilligramspercigarette,isgivenbytheequation: W (cid:1) (cid:2)(cid:1) m (cid:3) WS WB (cid:1)V W ES q where (cid:1) istheconcentrationofwaterinthesamplesmoketrap,inmilligramspermillilitre; WS (cid:1) istheconcentrationofwaterintheblanksmoketrap,inmilligramspermillilitre; WB q isthenumberofcigarettessmokedthrougheachsmoketrap; V isthevolumeofextractionsolventinwhichthecontentsofthesmoketrapweredissolved. ES Express the test results in milligrams per cigarette for each channel to the nearest 0,01mg, and the average per cigarettetothenearest0,1mg. 8 Repeatability and reproducibility A major international collaborative study involving 30laboratories and 6samples, conducted in 1990, showed that when cigarettes are smoked in accordance with ISO4387 and the resulting smoke solutions are analysed by this method,thefollowingvaluesfortherepeatabilitylimits(r)andthereproducibilitylimits(R)areobtained. The difference between two single results found on matched cigarette samples by one operator using the same apparatuswithintheshortestfeasibletimeintervalwillexceedtherepeatabilitylimit(r)onaveragenotmorethanonce in20casesinthenormalandcorrectoperationofthemethod. Single results on matched cigarette samples reported by two laboratories will differ by more than the reproducibility limit(R)onaveragenotmorethanoncein20casesinthenormalandcorrectoperationofthemethod. DataanalysisgavetheestimatesassummarizedinTable1. Table1—Estimatesgivenbydataanalysis Meanvalue Repeatabilitylimit Reproducibilitylimit m r R W mgpercigarette mgpercigarette mgpercigarette 0,083 0,154 0,241 0,153 0,228 0,353 0,338 0,272 0,381 0,962 0,407 0,734 1,595 0,561 0,935 3,187 0,908 1,680 4 IS 16042 (Part 1) : 2012 ISO 10362-1 : 1999 For the purpose of calculating r and R, one test result was defined as the mean yield obtained from smoking 20cigarettesinasinglerun. ForfurtherdetailsoftheinteractionofrandRwithotherfactors,seeCORESTAReport91/1. ThesubjectoftolerancesduetosamplingisdealtwithinISO8243. 9 Test report The test report shall give the water content per cigarette smoked and the method used, and shall include all conditions which may affect the result (e.g. atmospheric test conditions during smoking). It shall also give all details necessaryfortheidentificationofthecigarettessmoked. 5