Some standard content:
ICS55.020
National Standard of the People's Republic of China
GB/T14449—2008
Replaces GB/T14449—1993
Test method for aerosol products
Test method for aerosol productsIssued on 2008-07-18
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of ChinaStandardization Administration of the People's Republic of China
Implemented on 2009-01-01
This standard replaces GB/T14449—1993 "Test method for aerosol products". Compared with GB/T14449-1993, this standard has the following major changes: "net capacity, filling rate, leakage" has been added to the test content; the test temperature of internal pressure has been changed from 25℃±1℃ to the required temperature, with a temperature control accuracy of ±1℃"; GB/T14449-2008
has added two test methods to the flammability test, namely "closed space ignition test method" and "foam flammability test method"; the storage test method of aerosols has been modified; the test method of net capacity has been added; the test method of filling rate has been added; the test conditions of the test method of spray rate have been modified; the test of leakage rate has been deleted, and the test of leakage has been added. The flammability test method adopts the technical content of the aerosol test method in the United Nations "Recommendations on the Transport of Dangerous Goods: Manual of Tests and Criteria" (4th Edition), and other test methods refer to the standards of the American Society for Testing and Materials (ASTM). This standard is proposed by the China Packaging Federation. This standard is under the jurisdiction of the National Technical Committee for Packaging Standardization. The main drafting unit of this standard: Zhongshan Kaida Fine Chemical Co., Ltd. The participating drafting units of this standard: Shenzhen Rainbow Fine Chemical Co., Ltd., Guangzhou Botny Chemical Co., Ltd., Zhongshan Meijieshi Spray Valve Co., Ltd., Guangdong Laiya Chemical Co., Ltd., Taizhou Ludao Cosmetics Co., Ltd., Shanghai Johnson Co., Ltd., Hebei Kangda Co., Ltd., Shanghai Dazao Aerosol Co., Ltd., Zhongshan Lego Party Supplies Co., Ltd. The main drafters of this standard: Cui Ruping, Liang Peihui, Kang Zhenyu, Liang Weiming, Wang Xuemin, Li Yiqing, Ye Jianjun, Liu Ke, Wang Lu, Zheng Zhiyong, Ruan Shen, Liang Gaojian.
The previous versions of the standards replaced by this standard are: GB/T14449-1993.
1 Scope
Test methods for aerosol products
This standard specifies the basic test methods for aerosol products. This standard is applicable to the testing of aerosol products with a capacity of less than 1L. 2 Normative references
GB/T14449—2008
The clauses in the following documents become the clauses of this standard through reference in this standard. For all referenced documents with dates, all subsequent amendments (excluding errata) or revisions are not applicable to this standard. However, parties that reach an agreement based on this standard are encouraged to study whether the latest versions of these documents can be used. For all referenced documents without dates, the latest versions are applicable to this standard. Test method for ignition distance of sprays
GB/T21630—2008 Dangerous goods
GB/T21631-2008
Dangerous goods
GB/T21632—2008
Dangerous goods
Method for ignition of sprays in enclosed spaces
Test method for flammability of spray foam
BB/T0033 Classification and terminology of aerosol products 3 Terms and definitions
The terms and definitions determined in BB/T0033 apply to this standard. Test Contents
The following contents can be selected for various aerosol products: a) internal pressure;
flammability of spray mist;
stability of contents;
storability of container;
spray range;
spray angle;
particle size and distribution of mist particles;
spray rate;
amount of spray at one time;
spray rate;
net mass;
net capacity;
leakage;
filling rate.
5 Test method
5.1 Test of internal pressure
5.1.1 Instruments and test equipment
a) Pressure gauge: range 0MPa~1.6MPa, accuracy level 2.5, with special connector; b) Timer;
GB/T144492008
c) Constant temperature water bath: temperature control accuracy ±1℃, with metal frame clamp. 5.1.2 Test steps
Take three can samples and use the spray method indicated on the sample label to remove the propellant or air trapped in the valve and (or) straw during the filling operation; a)
Pull the sample out of the valve actuator and place it in a constant temperature water bath at the required temperature so that the water submerges the can body. The constant temperature time is not less than 30min; b)
Wear thick leather gloves and shake the sample six times (except for the sample marked that the can body is not allowed to be shaken), align the pressure gauge inlet with the valve stem, place the product upright, press hard, and record the pressure reading after the pressure gauge pointer stabilizes. Repeat the test three times for each can and take the average value: d) Test the second and third can samples in this way. The average value of the three test results is the internal pressure of the product. 5.2 Test of the flammability of spray mist
According to the properties of the product, the test shall be carried out in accordance with GB/T21630-2008, GB/T21631-2008GB/T21632--2008. 5.3 Test of the stability of contents
5.3.1 Preparation of samples
The containers and valves used for the samples shall be inspected and qualified; a)
After the containers and valves of the samples are sealed, the sealing diameter and depth shall be inspected and qualified; after being immersed in a 50℃ water bath, no bubbles shall be generated, and the internal pressure must be lower than the allowable operating pressure of the container and valve. e
5.3.2 Test conditions and sampling
a) The storage test at -17℃～0℃ is conducted for 4 weeks. Samples are taken and tested every week during the storage process. Each time, no less than 2 cans are taken. The total number of test samples is no less than 8 cans.
b) The storage test at 50℃±2℃ is conducted for 8 weeks. Samples are taken and tested every 2 weeks during the storage process. Each time, no less than 2 cans are taken. The total number of test samples is no less than 8 cans.
For the samples stored at -17℃～0℃ and 50℃, the samples should be allowed to return to room temperature before testing.c
The room temperature storage test is conducted for 1 year. Samples are taken and tested every quarter during the storage process. Each time, no less than 2 cans are taken. The storage environment temperature is recorded every week. The total number of test samples is no less than 8 cans. Note 1: When necessary, the above conditions can be selected with appropriate temperature or time according to the needs of different products. Note 2: If there are signs of corrosion or deformation of the container during the test, and the signs are confirmed after enlarged inspection, the test should be interrupted and the sample should be removed and processed in time to avoid accidents.
5.3.3 Test content
a) Test of physical and chemical performance indicators, including odor, color, phase, internal pressure and other physical and chemical indicators in the sample standard; b) Functional test, including the functional effect of the sample label and the functional indicator items in the sample standard. Evaluate the stability of the contents based on the test sample results. 5.4 Test of container storage stability
The storage test of aerosol products is divided into two tests: dynamic storage and static storage. 5.4.1 Preparation of samples
a) The containers and valves used for the samples shall be inspected and qualified; b) After the containers and valves of the samples are sealed, the sealing diameter and depth shall be inspected and qualified; after being immersed in a 50℃ water bath, no bubbles shall be generated within 3 minutes, and the internal pressure shall be lower than the allowable operating pressure of the container and valve; c)
d) For samples stored at non-room temperature, they shall be allowed to return to room temperature before being tested; e) The samples for each temperature storage test shall be divided into two groups in equal numbers, one group is numbered I and the other group is numbered II. Note 3: If there are signs of corrosion or deformation of the container during the test, and it is confirmed after the expanded inspection, the test shall be interrupted and the samples shall be removed and handled in time to avoid accidents.
5.4.2 Placement and storage form of samples The samples of groups I and II are placed upright and inverted in equal numbers. Group I is used for dynamic storage test, and group II is used for static storage test. 2
The upright type is used to examine the contact between the valve and the gas phase of the sample contents. The inverted type is used to examine the contact between the valve and the liquid phase of the sample contents. 5.4.3 Sample conditions and sampling
GB/T14449--2008
For the samples of the working group, take them out for testing every week during the purchase and storage period. Each test content shall be tested according to the test method specified in this standard. The samples of group II shall be taken out at the time specified in Table 1 and tested. Examples of test conditions and test requirements are shown in Table 1. Table 1 Example of storage test for aerosol products
Storage temperature
Storage placement
Number of fillings
Test period
Test rate
Number of cans used for each test
Test content
5.4.4 Test content
Dynamic storage
Room temperature, 36℃
Upright and inverted
24 (half inverted at each temperature)
Until completion
Leakage disk:
Internal pressure,
Spray rate (10s);
Particle size;
Inspection of door and can (when it cannot be used normally or for the last inspection).
Static storage
—1 Room temperature, 36℃54℃
Upright and inverted
144 (half inverted at each temperature)bzxz.net
1,3,6,12,18,24 months
24 (each temperature and each placement method)
Leakage volume;
Internal pressure;
Spray rate (10s);
Valve inspection;
Container inspection;
Content inspection.
a) Sealing performance test (this item is only used for group II samples) Determine the leakage during storage; b)
Test the spray rate and particle size:
Check the spray function of the valve and whether the metal, plastic, and rubber parts in the valve components are corroded, embrittled, softened, hardened, shrunk, over-expanded, and whether the tightness is normal; d) Check whether the container is deformed, and whether there are changes such as corrosion in various parts of the inner wall such as the top, bottom, gas phase and liquid phase position of the can body, deep gaps, and parts connected with the valve; e) The detection of the contents requires observing the changes in the color of the contents, whether there are sediments, and muddy substances. If corrosion is found or suspected, the moisture, iron content, and tin content of the product can be tested. Evaluate the storage resistance of the container based on the test results. 5.5 Spray range test
This method is applicable to spray-type aerosol products. 5.5.1 Apparatus
a) Base: length × width = 1000mm × 200mm; b) Scale: length 1000mm, scale 1mm, installed parallel to the top of the base, height adjustable; c) Constant temperature water bath: temperature control accuracy ±1℃, with metal frame clamp. 5.5.2 Test steps
a) Take three can samples, and follow the spraying method indicated on the sample to remove the propellant or air left in the valve and (or) straw during the filling operation; b) Place the sample in a 25℃ constant temperature water bath, immerse the can body in water, and keep the temperature constant for 30 minutes; Wear thick leather gloves, take out the sample, and wipe it dry. Except for the sample marked with "shaking of the can is not allowed", shake the sample six times; c) According to the spraying method marked on the sample, spray continuously for 1s at the scale zero of the ruler (three times of spraying can be used with a quantitative valve); keep the center line of the mist beam parallel and at the same height as the ruler during spraying, and record the scale of the center line of the mist beam at the beginning of the fall of the mist particles or the full flow. Repeat the test three times for each can and take the average value; e) Test the second and third cans of samples in this way, and the average value of the test results of the three cans is the spray range of the product. 5.5.3 Precautions a) There should be no open flames in the area during the test; b) The test should be carried out in a windless area; c) Ventilate and clean the device after the test. 5.6 Test of spray angle This method is applicable to spray-type aerosol products. 5.6.1 Test device
a) Single-phase AC motor: power 120W, speed 1400r/minb) Speed regulator: 1r/min~1400r/min;c) Connecting rod: used to connect the speed regulator with the rotating disk;d) Rotating disk: with a -60° fan-shaped notch, radius 150mm;e) Baffle: clamp 130mm×130mm kraft paper. 5.6.2 Preparation of samples
In order to record the fog type on the kraft paper, it is necessary to add appropriate dyes to the sample. The dyes can be added before filling, or an appropriate amount of dye solution can be injected through the valve. For products using polar solvents, gentian violet can be used, and for products using non-polar solvents, oil-soluble red can be used. When dyeing the emulsion, it is necessary to prevent the added substances from destroying the stability of the emulsion. 5.6.3 Test steps
a) Take three can samples and follow the spraying method indicated on the sample to remove the propellant or air trapped in the valve and (or) straw during the filling operation; b) Place the sample in a 25℃ constant temperature water bath, immerse the can in water, and keep the temperature constant for 30 minutes; Wear thick leather gloves, take out the sample and wipe it dry. Shake the sample six times, except for those marked that the can body is not allowed to be shaken; d) Position the sample so that the valve is aligned with the kraft paper, and the valve and the center of the kraft paper are on the same horizontal line. Adjust the distance between the valve and the kraft paper to ensure the best reception. For products with a larger spray angle, spray at a distance of 10cm to 15cm from the kraft paper, and for products with a smaller spray angle, spray at a distance of 15cm to 25cm from the kraft paper. Turn the turntable to move the fan-shaped notch away from the center of the kraft paper. Then start spraying and start the power to drive the turntable, so that the mist beam passes through the fan e
notch and sprays onto the kraft paper. Adjust the rotating disk speed to make the particle density sprayed on the kraft paper moderate to obtain a more complete mist pattern;) After the test, remove the kraft paper and measure the diameter of the overall pattern left by the spray beam on the paper and the distance from the sample to the paper. If necessary, the pattern can be photographed for later analysis. See Figure 1 for a schematic diagram of the test device: The second and third cans of samples are tested in this way, and the average of the test results of the three cans is the spray angle of the product. g
The spray angle is calculated according to formula (1):
a = 2arctg
Where:
aSpray angle;
dThe diameter of the overall pattern left by the spray beam on the paper, the diameter value is the average of the lengths of the pattern left by the spray beam on the paper in both the vertical and horizontal directions, in millimeters (mm);
The distance from the starting point of the spray beam to the kraft paper, in millimeters (mm). L
Repeat the test three times for each can and take the average value. 1 baffle;
2—kraft paper;
1 rotating disk;
1 connecting rod;
single-phase AC motor;
1 speed regulator;
sample.
5.7 Determination of particle size and distribution of mist particles
5.7.1 Method summary
Figure 1 Schematic diagram of test device
GB/T14449—2008
All small particles diffract light. This method uses laser as the light source. When the sprayed mist particles enter the laser beam, particles of different sizes diffract light at different angles. By using a silicon photodiode array detector to measure the intensity of diffracted light at different angles, the particle size and distribution characteristics of the mist particles can be measured.
5.7.2 Instruments
Laser diffraction particle size analyzer;
Constant temperature water bath: temperature control accuracy ±1°C, with metal frame clamp. Test steps
Take three can samples, spray according to the method indicated on the sample, and remove the propellant or air trapped in the valve and (or) straw during the filling operation; place the sample in a 25°C constant temperature water bath, immerse the can body in water, and keep the temperature constant for 30 minutes; wear thick leather gloves, take out the sample, and wipe it dry. Shake the sample six times, except for the sample marked that the can body is not allowed to be shaken; turn on the instrument according to the instrument operating procedures, select the appropriate lens according to the sample situation, and set the instrument's measurement parameters. Measure the background after the instrument stabilizes for 15 minutes;
Position the sample so that the center line of the spray mist beam is in the same plane as the laser beam and keeps it vertical, spray at different distances from the laser beam, and check the light shielding rate of the sample. When the shading rate reaches the range of 0.1 to 0.5, position the sample; f
Spray the sample again for 5S, measure the result, repeat the test three times for each can, and take the average value; g) Test the second and third cans of samples in this way, and the average value of the test results of the three cans is the particle size of the mist particles of the product. 5.7.4 Report
The result report is given in the form of a histogram and a list. In addition to listing the particle size distribution data, the tabular result is also required to give the mass median particle size D (V.0.5). The result report should indicate the focal length of the lens, the length of the mist particles crossing the laser beam, the shading rate, the calculation mode and parameters, etc. At the same time, it is also necessary to record the distance from the laser beam to the valve.
5.8 Test of ejection rate
5.8.1 Instruments
a) Stopwatch: accuracy 0.2s;
b) Constant temperature water bath: temperature control accuracy ±1°C, with metal rack clamp. 5.8.2 Test steps
a) Take three cans of samples and use the spray method indicated on the sample label to remove the propellant or air trapped in the valve and (or) straw during the filling operation; place the sample in a 25℃ constant temperature water bath, immerse the can in water, and keep the temperature constant for 30 minutes; b)
c) Wear thick leather gloves, take out the sample, and wipe it dry; d) Weigh mi (accurate to 0.01g);
Except for the sample marked that the can body is not allowed to be shaken, shake the sample six times and accurately press the valve (fully open) actuator. If the net capacity is less than e
or equal to 400mL, press the valve actuator for 5s; if the net capacity is greater than 400mL, press the valve actuator for 10s. Then wipe off the liquid on the surface of the sample and weigh it to get mz (accurate to 0.01g); the spray rate (X,) is calculated according to formula (2):
Xi=m)-m2
Where:
Xr——spray rate, in grams per second (g/s); m-
——sample mass before spraying, in grams (g); m-
——sample mass after spraying, in grams (g); m2
tactual spray time, in seconds (s). Repeat the test three times for each can and take the average value. f) Test the second and third samples in the same way. The average value of the test results of the three cans is the spray rate of the product. 5.9 Test of single spray volume
Applicable to aerosol products with quantitative valves. 5.9.1 Instrument
Balance: The graduation value shall not be less than 0.01g.
5.9.2 Test steps
Take 4 bottles of test samples, remove the caps, test spray several times with the pressure valve removed, wipe clean, accurately weigh, lift the pressure valve to spray once, wipe clean, and accurately weigh again. The difference between the two weights is 1 spray volume. Measure 3 spray volumes continuously according to the above method; spray 10 times continuously without weighing the weight of the pressure valve removed: then measure 3 spray volumes continuously according to the above method; spray 10 times continuously without weighing the weight of the pressure valve removed, and finally measure 4 spray volumes continuously according to the above method. Calculate the average of the 10 spray volumes for each bottle. 5.10 Test of spray rate
5.10.1 Instrument
Constant temperature water bath: temperature control accuracy ±1℃, with metal rack clamp. 5.10.2 Test steps
a) Take three cans of samples and place them in a 25℃ constant temperature water bath, immerse the cans in water, and keep the temperature constant for 30 minutes; b) Wear thick leather gloves, take out the samples, and wipe them dry. Weigh and get ms (accurate to 0.1g); Except for the samples that do not allow shaking of the can body, shake the sample six times and spray the contents according to the spray method indicated on the sample until no more contents are sprayed out, and weigh and get m (accurate to 0.1g); open the can and remove the residue, and then weigh the sample mass (empty can and components, such as glass beads, etc.) to get ms (accurate to 0.1g); d)
Test the second and third cans of samples in this way. , the average of the three can test results is the spray rate of the product; e)
The spray rate (X,) is calculated according to formula (3): 6
Where:
X——spray rate,%;
m3-m×100
Total mass of the sample, in grams (g);
Mass of the sample after spraying, in grams (g):
msMass of the empty can and components, in grams (g). Note 4: The spraying is carried out in a fume hood.
Note 5: If the temperature is too low during the test, it can be put back in a 25°C water bath for a while and then continue to spray. 5.11 Test of net mass
5.11.1 Instrument
Balance: The graduation value shall not be less than 0.01g.
5.11.2 Test steps
GB/T14449—2008
（3）
Take three cans of samples, weigh them and get m6, then spray the contents according to the spraying method indicated on the sample, open a hole in the can after spraying and remove the remaining liquid, and then weigh the sample mass (empty can and components) to get m. The net mass (X,) is calculated according to formula (4): X, mgm
Where:
X;——net mass, in grams (g); mg
——total mass of the sample, in grams (g); mass of the sample after removing the remaining liquid, in grams (g). Test the second and third cans of samples in this way, and the average of the three can test results is the net mass of the product. 5.12 Test of net capacity
This method is not applicable to gas labor products using quantitative valves and valves with gas phase bypass holes. 5.12.1 Apparatus
a) A graduated glass aerosol test tube, with a capacity of 90 mL and a minimum graduation value of 1 mL; b) A balance: the graduation value shall not be less than 0.01 g. 5.12.2 Test steps
Take the sample and weigh its mass ms. Assemble the glass aerosol test tube, and pay attention to using a valve without a straw. Fill the glass test tube with 10 mL of LPG through a plastic tube about 8 mm long and with an inner diameter slightly smaller than the diameter of the sample valve stem (the aerosol valve straw can be used). Then install the nozzle and spray the LPG until no gas comes out to take away the air in the test tube. Weigh its mass m. First, shake the sample thoroughly, then use a plastic tube to connect the valve stems of the sample and the glass test tube, with the glass aerosol test tube on top and the sample on the bottom. Press with appropriate force to connect the sample and the glass test tube. At this time, the contents should be injected into the glass test tube from the sample. When the injected contents account for 65% to 80% of the volume of the glass test tube, stop pressing, remove the sample, weigh the mass m1g of the glass aerosol test tube, place the glass aerosol test tube in an environment of 25℃±2℃ for 30min, and read the liquid level scale V after the liquid level of the contents stabilizes. Then measure the net mass X3 of the sample according to 5.11. See Figure 2 for the test device diagram. 5.12.3 Calculation
Net capacity (X,) is calculated according to formula (5):
Wherein:
X, is the net capacity, in milliliters (mL); mg
mio-mg
The mass of the empty glass aerosol test tube, in grams (g); XV
（5）
GB/T14449-2008
The mass of the glass aerosol test tube after the sample content is filled, in grams (g); X: —The net mass of the sample, in grams (g); V —The volume of the sample filled into the glass aerosol test tube, in milliliters (mL). Glass aerosol test tube
Plastic tube
Figure 2 Net capacity measurement device diagram
5.13 Test of leakage disk
The leakage test is carried out at two storage temperatures. 5.13.1 Instrument
Balance: precision is 0.01g.
5.13.2 Test steps
5.13.2.1 Leakage during storage at room temperature
Take 10 to 20 cans as samples and, according to the spraying method indicated on the sample label, remove the propellant or air trapped in the valve and (or) straw during the filling operation. Then weigh them separately to obtain m12. After storing at room temperature for a specified time, take them out and weigh them separately to obtain m13. The leakage (Xs) is calculated according to formula (6):
Xs=m12-mis
Where:
X——leakage, in grams (g);
m12—the mass of each can before storage at room temperature, in grams (g); m13
the mass of each can after storage at room temperature, in grams (g). The average value of the test results is the leakage of the product within the specified storage time. 5.13.2.2 High-temperature storage leakage
Take 10 to 20 cans as samples and remove the propellant or air trapped in the valve and (or) straw during the filling operation according to the spraying method indicated on the sample. Then weigh them separately to obtain m1. After storing them at an ambient temperature of 50℃±2℃ for 3 months, take them out and weigh them separately to obtain m15. Leakage X. Calculate according to formula (7):
X=mu-mis
Where:
-leakage, in grams (g);
The mass of each can before high-temperature storage, in grams (g); (7)
The mass of each can after high-temperature storage, in grams (g). The average value of the test results is the leakage of the product stored at 50℃±2℃ for 3 months. The test temperature and time can be determined according to different requirements. 5.14 Filling rate test
5.14.1 Instrument
a) Apparatus see 5.12 Net capacity test;
b) Balance: accuracy is 0.01g.
5.14.2 Test steps
GB/T14449—2008
Take the sample and weigh its mass mg. Assemble the glass aerosol test tube, pay attention to using a valve without a straw, fill the glass test tube with 10mL of petroleum gas through a plastic tube about 8mm long and with an inner diameter slightly smaller than the diameter of the sample valve stem (the aerosol valve straw can be used), then install the nozzle and spray the petroleum gas until no gas comes out to take away the air in the test tube, and weigh its mass mg. First, shake the sample thoroughly, then use a plastic tube to connect the valve stem of the sample and the glass test tube, with the glass aerosol test tube on top and the sample on the bottom. Press with appropriate force to connect the sample and the glass test tube. At this time, the contents should be injected from the sample into the glass test tube. When the injected contents account for 65% to 80% of the volume of the glass test tube, stop pressing, remove the sample, weigh the mass m10 of the glass aerosol test tube, place the glass aerosol test tube in an environment of 25℃±2℃ for 30 minutes, and read the liquid level scale V after the liquid level is stable. Then measure the net mass X of the sample according to the provisions of 5.11. Add 25℃ water to the empty can until it is full, put the glass beads and valves and other components into the can, absorb the water outside the can and weigh m16.
Filling rate X, calculated according to formula (8).
In the formula:
Filling rate, %;
X0.9977×100
The mass of the sample after removing the residual liquid, in grams (g); the mass of the empty glass aerosol test tube, in grams (g); the mass of the glass aerosol test tube after the sample content is filled, in grams (g); the total mass of the empty tank after water is injected, in grams (g); the net mass of the sample, in grams (g); the volume of the sample injected into the glass aerosol test tube, in milliliters (mL); the density of water at -25℃, in grams per milliliter (g/mL). The constant temperature and time of the test can be determined according to the requirements of different products. -（8）
GB/T14449-2008
People's Republic of China
National Standard
Test Method for Aerosol Products
GB/T14449-—2008
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