CN104833608A - Method for determining overall migration of tipping paper for cigarette - Google Patents

Abstract

A method for determining overall migration of tipping paper for a cigarette is characterized by including enabling a sample of the tipping paper for the cigarette to be in immersed contact with simulant water according to specific time, a specific temperature and a specific contact proportion, then transferring a simulated solution to an evaporation pan prior to evaporating to dryness, and calculating residue mass by a weight difference method so as to obtain the overall migration of the tipping paper for the cigarette by taking the water as a simulant. The method for determining the overall migration of the tipping paper for the cigarette is capable of simulating a mouth cavity and cigarette contact process and accurately determining the total mass of non-volatile matter migrated from the tipping paper for the cigarette to the simulant water.

Description

A kind of assay method of cigarette tipping paper gross migration

Technical field

The invention belongs to the physical and chemical index analysis technical field of smoking material, be specifically related to a kind of assay method of cigarette tipping paper gross migration.Utilize the method can the contact process of Mouthsimulator and cigarette, the nonvolatile matter gross mass that Accurate Determining cigarette tipping paper moves out in analogies water.

Background technology

Gross migration limitation (overall migration limit, OML) refers to the maximum magnitude being released into nonvolatile matter food simulants from food contact material or goods.This index is derived from the General Requirement that European Union (EC) No 1935/2004 decree " about intending with the material of Food Contact and goods and abolishing 80/590/EEC and 89/109/EEC instruction " framework regulation proposes food contact material; that is: " under normal or foreseeable service condition; its composition must not jeopardize human health to the migration amount in food; or cause the unacceptable change of food composition, or cause the deterioration of food organoleptic attribute.”

For implementing this clause, European Union Res AP (2004) 1 resolves (about intending the coating with Food Contact) and (EU) No 10/2011 regulation (about intending and the plastic material of Food Contact and goods) all proposes gross migration≤10 mg/dm ²restriction requirement.Cigarette tipping paper touches material as mouth, and in consumer's smoking cigarette process, tipping paper surface mass is likely moved by saliva contacts, and the assay method therefore setting up migration amount for cigarette tipping paper is conducive to improving cigarette tipping paper product quality.And according to literature survey, at present both at home and abroad, there is no patent and the bibliographical information of cigarette tipping paper gross migration method of testing.

Summary of the invention

Object of the present invention for the technological gap of cigarette tipping paper gross migration test, proposes a kind of method of testing of cigarette tipping paper gross migration just.

The object of the invention is to be achieved through the following technical solutions: cigarette tipping paper sample is carried out submergence contact with analogies water according to the time specified, temperature and the ratio of contact, afterwards simulated solution is transferred to evaporating dish and evaporate to dryness, utilize the heavy method of difference to calculate the quality of residue, draw with water to be the gross migration of analogies cigarette tipping paper.

Method of testing of the present invention comprise sample preparation, submergence contact, simulated solution evaporation, migration quality testing survey four steps.Specific as follows:

1, sample preparation: sample is cut into 50 ~ 200 cm ²sample (Width all counts, length variation should within ± 1 mm), and perforation hangs on bracing frame.

2, submergence contact: according to 1 cm ²the contact gear ratio of sample contacts 1 mL water, the water getting respective volume is placed in glass test tube, balances 10 ~ 20 min, the bracing frame hanging with sample is placed in glass test tube in 40 DEG C of water-baths, submergence contact 30 ~ 31 min.

3, move quality testing to survey: after submergence contact test terminates, the bracing frame hanging with sample is shifted out from glass test tube, and allow the current that sample and sample mount are adhered to be back in glass test tube.Simulated solution is poured out in evaporating dish, then evaporating dish is placed in heating evaporation on heating plate.When evaporation is near dry, evaporating dish is put into baking oven 30 min of (105 ± 1) DEG C, make the complete evaporate to dryness of water.Add a cover taking-up evaporating dish, put into exsiccator and be cooled to room temperature (about 30 min), electronic balance weighing (sensibility reciprocal 0.1 mg).Evaporating dish is reentered into baking oven, repeats aforesaid operations, until twice weighing result change is no more than 0.5 mg.

4, result calculates and statement

Cigarette tipping paper gross migration calculates by formula (1):

……………………（1）

In formula:

m---gross migration, unit is milligram every square decimeter (mg/dm ²);

m _a0 ---sample evaporation ware quality before migration test, unit is gram (g);

m _a1 ---sample evaporation ware quality after migration test, unit is gram (g);

m _b0 ---blank evaporating dish quality before migration test, unit is gram (g);

m _b1 ---blank evaporating dish quality after migration test, unit is gram (g);

s---sample cutting area, unit is square decimeter (dm ²).

Using the difference of the arithmetic mean of the arithmetic mean of three replicate determinations and twice blank determination as measurement result, be accurate to 0.1 mg/dm ².

The absolute deviation of parallel determinations and three replicate determination arithmetic mean should be less than 1 mg/dm ².

5, method " recovery "

The simulated experiment of table 1 recovery

In order to examine or check the confidence level of method, with reference to the design concept of the recovery test that instrumental analysis is commonly used, utilize NaCl inorganic salts as gross migration " simulant standard samples ", by add " simulant standard samples " of known quantity in the soak solution after migration after, carry out subsequent measurements, and calculate the recovery.By this experiment, can the experimental error of verification method in the evaporation of simulated solution, drying, balance and mensuration process, investigation method confidence level.This test have chosen the tipping paper sample of 3 contents levels, adds the simulant standard samples of different mark-on level respectively, learns by testing and calculating, and the recovery, between 80.0% to 112.7%, illustrates that this method has higher accuracy (table).

6, method precision

Table 2 r, rdata

Gross migration measurement result	Repeatability limit ( r）	Repeatability limit ( R）
			6.7 mg/dm 2	1.3 mg/dm 2	1.7 mg/dm 2

According to the requirement of EN 1186-1:2002, carried out 1 sample repeatability limit ( r), repeatability limit ( r) investigate.According to GBT 6379.2-2004 " the accuracy part 2 confirmed standard measuring method repeatability of measuring method and result and the basic skills of repeatability " standard, spatial pattern and process is utilized to check each laboratory data outlier, Charles Dixon is utilized to check the outlier of each laboratory mean value, utilize the outlier of the precision test variances such as Ke Kelun, calculate after outlier is rejected r, r.By calculating, gross migration is at 6.7 mg/dm ²sample, repeatability limit rand repeatability rbe respectively 1.3 mg/dm ²with 1.7 mg/dm ²(table 2).

The invention has the advantages that can simulate cigarette tipping paper and oral contact process when smoking, the nonvolatile matter gross mass that Accurate Determining cigarette tipping paper moves out in analogies water.And test result accurately and reliably, reproducible, device therefor is easy to obtain, simple to operate.

Accompanying drawing explanation

Fig. 1 is support frame structure schematic diagram used herein.

Embodiment

The present invention is further described with following experimental data and Fig. 1:

One, cigarette tipping paper sample to be measured: 6, comprises 4 kinds of mode of printings.

Two, material and instrument

Shear plate, totally level and smooth glass, metal or plastic board, its area should for the preparation of sample; Crop tool, scissors, blade or other suitable tools; Electronic balance: sensibility reciprocal 0.1 mg; Water, meets the requirement of secondary water in GB/T 6682; Moving apparatus: tool grinding port plug glass tube, internal diameter 30 mm, not containing ground length about 170 mm.Bracing frame, glass material; Water bath with thermostatic control, controls for migration test temperature; Evaporating dish, tool ground lid.Diameter about 60 mm, deeply about 30 mm, quality is no more than 100 g; Heating plate, for the evaporation of analogies (water); Exsiccator, with automatically indicating silica gel; 100 mL graduated cylinders.

Three, method step

1, sample preparation.Sample is cut into 100 cm ²sample (Width all counts, length variation should within ± 1 mm), and perforation hangs on bracing frame (see Fig. 1).

2, submergence contact.The glass test tube filling 100 mL water is balanced in 40 DEG C of water-baths, after the bracing frame hanging with sample is placed in glass test tube 30 min, sample should be immersed in water completely, and fully contacts.

3, move quality testing to survey.

1) evaporating dish prepares

After 5 numbered clean evaporating dish uncaps, together put into baking oven, at (105 ± 1) DEG C, place 30 min.Add a cover taking-up evaporating dish, put into exsiccator and be cooled to room temperature (about 30 min), weigh, be accurate to 0.1 mg.Evaporating dish is reentered into baking oven, repeats aforesaid operations, until twice weighing result change is no more than 0.5 mg.

2) evaporate

After submergence contact test terminates, the bracing frame hanging with sample is shifted out from glass test tube, and allow the current that sample and sample mount are adhered to be back in glass test tube.Pour out about 50 mL water to evaporating dish from 5 glass test tubees respectively, then evaporating dish is placed in heating evaporation on heating plate (attention is avoided causing damage because of boiling or splashing).When evaporation is closely dry, pours corresponding evaporating dish into by often propping up glass test tube residue water, and pour in the lump for 2 times with 10 mL water rinse glass test tubees.When evaporation is near dry, evaporating dish is put into baking oven 30 min of (105 ± 1) DEG C, make the complete evaporate to dryness of water.Add a cover taking-up evaporating dish, put into exsiccator and be cooled to room temperature (about 30 min), weigh, be accurate to 0.1 mg.Evaporating dish is reentered into baking oven, repeats aforesaid operations, until twice weighing result change is no more than 0.5 mg.Be as the criterion with last weighing result.

The gross migration result of 6 samples calculates, specifically in table 3 by formula (1).

Table 3 tipping paper sample gross migration test result

Sample number into spectrum	Gross migration (mg/m 2）
		J1	4.1
J2	2.7
		J3	7.4
J4	2.8
		J5	1.9
J6	3.4

Claims (2)

1. the assay method of a cigarette tipping paper gross migration, it is characterized in that: cigarette tipping paper sample is carried out submergence contact with analogies water according to the time specified, temperature and the ratio of contact, afterwards simulated solution is transferred to evaporating dish and evaporate to dryness, the heavy method of difference is utilized to calculate the quality of residue, draw with water to be the gross migration of analogies cigarette tipping paper, concrete steps are as follows:

1) sample preparation: cigarette tipping paper sample is cut into 50 ~ 200 cm ²sample, and perforation hangs on bracing frame, tipping paper Width all counts, and length variation should within ± 1 mm;

2) submergence contact: according to 1 cm ²the contact gear ratio of sample contacts 1 mL water, the water getting respective volume is placed in glass test tube, balances 10 ~ 20 min, the bracing frame hanging with sample is placed in glass test tube in 40 DEG C of water-baths, submergence contact 30 ~ 31 min ;

3) move quality testing to survey: after submergence contact test terminates, the bracing frame hanging with sample is shifted out from glass test tube, and allow the current that sample and sample mount are adhered to be back in glass test tube, simulated solution is poured out in evaporating dish, then evaporating dish is placed in heating evaporation on heating plate, when evaporation is closely dry, evaporating dish is put into baking oven 30 min of 105 ± 1 DEG C, make the complete evaporate to dryness of water; Add a cover taking-up evaporating dish, put into exsiccator and be cooled to room temperature, electronic balance weighing; Evaporating dish is reentered into baking oven, repeats aforesaid operations, until twice weighing result change is no more than 0.5 mg;

4) gross migration calculates: using containing the quality after migration thing evaporating dish evaporate to dryness and the blank evaporating dish ratio with the sample area of poor quality gross migration as cigarette tipping paper, and unit is mg/dm ².

2. the assay method of cigarette tipping paper gross migration according to claim 1, is characterized in that: the specific formula for calculation that gross migration calculates is as follows:

Calculate:

……………………（1）

In formula:

m---gross migration, unit is milligram every square decimeter (mg/dm ²);

m _a0 ---sample evaporation ware quality before migration test, unit is gram (g);

m _a1 ---sample evaporation ware quality after migration test, unit is gram (g);

m _b0 ---blank evaporating dish quality before migration test, unit is gram (g);

m _b1 ---blank evaporating dish quality after migration test, unit is gram (g);

s---sample cutting area, unit is square decimeter (dm ²);

Using the difference of the arithmetic mean of the arithmetic mean of three replicate determinations and twice blank determination as measurement result, be accurate to 0.1 mg/dm ²;

The absolute deviation of parallel determinations and three replicate determination arithmetic mean should be less than 1 mg/dm ².