CORESTA RECOMMENDED METHOD N 68

Transcription

1 COESTA ECOMMENDED METHOD N 68 DETEMINATION OF CABON MONOXIDE IN THE MAINSTEAM SMOKE OF CIGAS BY NON-DISPESIVE INFAED ANALYSIS (Januay 2010) 1. FIELD OF APPLICATION The method is applicable to the gas phase of the mainsteam smoke of cigas. 2. DEFINITIONS 2.1. The gas phase of ciga smoke is that pat of the mainsteam smoke which passes though a smoke tap confoming to COESTA ecoended Method N A cleaing puff is any puff taken afte the ciga has been extinguished, with the same volume as dawn while smoking. 3. EFEENCES COESTA ecoended Method N 46 : 1998 Atmosphee fo Conditioning and Testing Cigas of all Sizes and Shapes. COESTA ecoended Method N 64 : 2005 outine Analytical Ciga-Smoking Machine - Specifications, Definitions and Standad Conditions. COESTA ecoended Method N 65 : 2010 Detemination of Total and Nicotine-Fee Dy Paticulate Matte using a outine Analytical Ciga-smoking machine - Detemination of Total Paticulate Matte and Pepaation fo Wate and Nicotine Measuements. COESTA ecoended Method N 47 : 2000 Cigas - Sampling 4. PINCIPLE Cigas ae smoked accoding to a standadised pocedue. The cabon monoxide of the total gas phase of the smoke is detemined by non-dispesive infaed analysis

2 5. APPAATUS 5.1. A standad smoking machine with accessoies complying with COESTA ecoended Method N A system fo the collection of the total gas phase satisfying the following conditions: It must not intefee with the nomal pefomance of the smoking machine and, consequently, with the detemination of total paticulate matte and nicotine It must be constucted and maintained so that the cabon monoxide content of the gas phase sample of ciga smoke containing appoximately 5 v/v (4-6 v/v) of cabon monoxide does not change by moe than 0.3 v/v CO ove a peiod of thee hous Its volume must be chosen accoding to the actual smoking conditions and must be at least equal to the final volume of the gas phase plus cleaing puffs but it is ecoended that it does not exceed twice that final volume. In pactice the collection of the gas phase fom cigas equies a volume, that depends on the size of the ciga and the coesponding puff volume (see CM 65, paagaph ). Depending on the cabon monoxide equipment s specifications, a minimum gas phase volume could be equied fo a measuement. To meet this equiement the collection of the gas phase of moe than one ciga, smoked in the same o in diffeent channels, could be needed A non-dispesive infaed analyse satisfying the manufactue s instuctions and the following conditions : ange of measuement: An instument of sufficient ange to accoodate expected sample values, which can depend on the numbe of cleaing puffs used to dilute the sample. Fo undiluted gas samples a ange of 0.00 v/v to v/v has been detemined to be sufficient. Altenative anges ae acceptable povided that the pefomance specification given in paagaph is equalled o exceeded Pecision: Lineaity: esolution: +/ v/v o bette +/ v/v o bette 0.01 v/v o bette epeatability: +/ v/v o bette, detemined ove the nomal measuement peiod and unde conditions of constant tempeatue and pessue Its esponse to 10 (v/v) of cabon dioxide must not exceed 0.05 (v/v) as cabon monoxide. Its esponse to 2 (v/v) of wate vapou must not exceed 0.05 (v/v) as cabon monoxide A themomete fo measuing ambient tempeatue to the neaest 0.2 C A baomete fo measuing atmospheic pessue to the neaest 0.1 kpa

3 6. STANDAD GASES At least thee standad gas mixtues of accuately known concentations of cabon monoxide in nitogen coveing the expected ange in such a way as to avoid extapolation of the calibation cuve; typically 2, 7 and 12 (v/v) of cabon monoxide in nitogen, o any othe set of 3 standads accoding to the specified ange of the CO analyze. The concentations must be guaanteed by the supplie to be bette than 2 (elative). Note : Make up gases othe than nitogen, such as helium, must not be used as the detecto esponse fo cabon monoxide will be diffeent. 7. SAMPLING AND SAMPLE PEPAATION 7.1. The sampling of cigas must be caied out accoding to COESTA ecoended Method N The sample fo smoking must be conditioned accoding to COESTA ecoended Method N Calibation of the analyse 8. POCEDUE Afte waming up the instument accoding to the manufactues ecoendations, puge the instument with ai and adjust to ead zeo Fill a peviously evacuated gas phase collection containe with the standad gas of nominally 12 CO (v/v), o anothe concentation close to the uppe limit of the equipment ange, e-evacuate and efill with gas. Ensue that the gas in the containe is at ambient tempeatue and pessue. Intoduce the gas into the measuing cell of the analyse using the system sampling pump. Note the value when a steady eading has been obtained If necessay, adjust the instument eading to agee with the cetified value of the standad gas epeat fo the othe standad gases. If thee is a diffeence geate than 0.3 CO (v/v) between the obseved and expected values, attention should be given to the analyse lineaity Establish the elationship between the eadings and the actual cabon monoxide concentations in the standad gases at least weekly. This must be linea within the limits epoted in section 5. Non lineaity indicates that thee is an instument poblem Check the calibation pio to measuement using the standad gas containing about 12 (v/v) cabon monoxide), o anothe concentation close to the uppe limit of the equipment ange. If thee is a diffeence geate than 0.3 CO (v/v) between obseved and expected values epeat the full calibation (8.1.)

4 8.2. Smoking and collection of gas phase Setting up the gas phase collection system. Poceed in accodance with the instuctions petinent to the equipment used. In paticula ensue that the collection device is popely evacuated befoe the stat of smoking. Thee must not be any esidual vacuum upsteam of the collection device befoe smoking Smoking pocedue Set up the smoking machine in accodance with COESTA ecoended Method N 64 and smoke the cigas in accodance with COESTA ecoended Method N Afte the completion of the smoking of each ciga emove the buning coal of the ciga butt and take the necessay cleaing puffs -at least one- to assue that all gas phase has been collected and that the CO measuement ( (v/v)) is within the equipment s specified ange (see COESTA ecoended Method N 65, paagaph ). To fulfil this equiement the numbe of cleaing puffs (dilution pocess) must be adjusted accoding to the expeience with pevious measuements in simila samples. Then emove the ciga butt ecod the total numbe of puffs taken on each channel, i.e. smoking puffs plus cleaing puffs Measuement of the cabon monoxide content of the collected gas phase echeck the calibation of the analyse (see ) and intoduce the gas phase into the measuing cell of the analyse unde the same conditions of sampling and ambient tempeatue and pessue and the same gas flow ate as used duing calibation. ead the analyse output and detemine the obseved cabon monoxide concentation At the end of each smoking the gas phase collection containe must be emptied. The appaatus is then eady fo the next smoking stating at CALCULATIONS 9.1. Let : C obs = obseved cabon monoxide concentation, (v/v) N = total numbe of puffs in the measued sample (including cleaing puffs) q = numbe of cigas smoked to poduce the measued sample V = puff volume, ml t = ambient tempeatue, C p = ambient pessue, kpa W = aveage mass of conditioned cigas, g pe ciga - 4 -

5 9.2. Calculation of cabon monoxide yield - mass pe ciga basis. mg cabon monoxide pe ciga = Cobs x V x N x p x 273 x 28 q x 100 x x ( t+273) x Calculation of cabon monoxide yield mass pe gam tobacco basis. C obs x V x N x p x 273 x 28 mg cabon monoxide pe gam tobacco = q x 100 x x (t+273) x 22.4 x W 10. TEST EPOT The test epot shall show the method used and the esults obtained. It shall also mention any opeating conditions not specified in this ecoended Method, o egaded as optional, as well as any cicumstances that may have influenced the esults. The test epot shall include all details equied fo complete identification of the sample. Whee appopiate, ecod the infomation in to Chaacteistic data about the ciga Ciga identification - in the case of a coecial ciga this should include : a) Name of manufactue, county of manufactue; b) Poduct name; c) Date of sampling; d) Place of puchase o sampling; e) Kind of sampling point; f) Sampling point (e.g. addess of etail outlet o machine numbe); g) Packet numbe (of that poduct sampled that day); h) Maks on any tax stamp; i) Length of ciga; j) Whee applicable : length of filte; k) Whee applicable : length of atificial mouthpiece Sampling a) Type of sampling pocedue; b) Numbe of cigas in laboatoy sample; c) Date and location of puchase Desciption of test a) Date of test; b) Type of smoking machine used; c) Type of analyse used; d) Total numbe of cigas smoked in the entie detemination on that ciga type; e) Numbe of cigas smoked into each gas collection device; - 5 -

6 f) Butt length; g) oom tempeatue ( C) duing smoking opeation and analysis; h) elative humidity () duing smoking opeation; i) Atmospheic pessue (kpa) duing smoking opeation and analysis Test esults. The expession of the laboatoy data depends on the pupose fo which the data ae equied, and the level of laboatoy pecision. Confidence limits shall be calculated and expessed on the basis of the laboatoy data befoe any ounding has taken place. a) Aveage length of the cigas to the neaest 0,5 ; c) Aveage length of the filte (whee applicable) to the neaest 0,5 ; c) Aveage length of the tip (whee applicable) to the neaest 0,5 ; d) Butt length to which the cigas wee smoked to the neaest 0,1 ; e) Aveage length of tobacco potion smoked to the neaest 0,1 ; f) Aveage diamete of the cigas at 15 fom mouth end, to the neaest 0,1 (fo the detemination of the holde constuction); g) Aveage diamete of the cigas at 33 fom mouth end, to the neaest 0,1 (fo the detemination of the Puff Volume); h) Aveage daw esistance of the conditioned cigas; i) Aveage mass (mg pe ciga) of the conditioned cigas selected fo the smoking opeation; j) Wate content ( mass/mass) of the conditioned cigas; k) Aveage numbe of puffs pe ciga fo each channel to the neaest 0,1 puff; l) Aveage numbe of total puffs taken fo each channel/collection device including final cleaing puffs to the neaest 0,1 puff; m) Obseved cabon monoxide concentation ( v/v) fo each channel to the neaest 0,01; n) Cabon monoxide (mg pe ciga) fo each channel to the neaest 0,1 mg and the aveage pe ciga to the neaest 1 mg; o) Cabon monoxide (mg pe gam tobacco) fo each channel to the neaest 0,1 mg, dividing the Cabon monoxide (in mg/ciga) by the ciga mass (in g pe ciga) of the conditioned cigas selected fo smoking in each paticula channel, and the aveage pe gam tobacco to the neaest 1 mg. 11. EPEATABILITY AND EPODUCIBILITY A Collaboative Study involving 7 laboatoies conducted in 2008/2009 shows the following values fo epeatability () and epoducibility () of this method. The diffeence between two single esults found on matched ciga samples by one opeato using the same appaatus within the shotest feasible time inteval will exceed the epeatability value () on aveage not moe than once in 20 cases in the nomal and coect opeation of the method. Single esults on matched ciga samples epoted by two laboatoies will diffe by moe than the epoducibility () on aveage not moe than once in 20 cases in the nomal and coect opeation of the method

7 Data analysis gave the estimates (expessed in mg/ciga) as suaised in the following table 1: Poduct weight diamete length CO g mg/ciga mg/ciga mg/ciga A 0,97 7,9 84,0 11,12 1,74 3,07 15,65 27,62 B 0,73 7,5 70,0 23,06 3,16 5,71 13,70 27,78 C 2,00 10,3 96,0 60,66 5,47 8,60 9,01 14,17 D 5,80 15,4 114,5 190,16 27,84 60,35 14,64 31,73 E 13,30 18,1 194,0 475,42 108,86 175,24 22,90 36,86 Data analysis gave the estimates (expessed in mg/g) as suaised in the following table 2: Poduct weight diamete length CO g mg/g mg/g mg/g A 0,97 7,9 84,0 11,50 1,75 3,10 15,22 26,96 B 0,73 7,5 70,0 32,08 4,19 7,51 13,06 23,40 C 2,00 10,3 96,0 31,66 2,56 5,15 8,09 16,26 D 5,80 15,4 114,5 33,33 5,00 10,27 14,99 30,82 E 13,30 18,1 194,0 35,93 9,47 14,32 26,36 39,84 Fo the puposes of calculating and, one test esult (o one single esult) was defined as the mean yield obtained fom smoking 8 cigas. The subject of toleances due to sampling is dealt with in COESTA ecoended Method N 47 : (CO = Cabon Monoxide) - 7 -