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GB 24330-2009 PDF in English


GB 24330-2009 (GB24330-2009) PDF English
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GB 24330-2009: PDF in English

GB 24330-2009
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 65.100.10
G 25
General security technical specification for domestic
sanitary insecticide
ISSUED ON: SEPTEMBER 30, 2009
IMPLEMENTED ON: MAY 01, 2010
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Terms and definitions ... 4 
4 Requirements ... 5 
5 Test methods ... 8 
Annex A (normative) Method for determining content of active ingredients in
mosquito coils ... 14 
Annex B (normative) Method for determining content of active ingredients in
electrothermal mosquito tablet incense ... 17 
Annex C (normative) Method for determining content of active ingredients in
electrothermal mosquito liquid incense ... 20 
Annex D (normative) Method for determining content of active ingredients in
insecticide aerosol ... 23 
Annex E (normative) Method for determining amount of soot of mosquito coil
... 28 
General security technical specification for domestic
sanitary insecticide
1 Scope
This Standard specifies general terms and definitions, requirements, test
methods of domestic sanitary insecticide.
This Standard is applicable to general requirements related to health,
environmental safety of domestic sanitary insecticide.
2 Normative references
The provisions in following documents become the provisions of this Standard
through reference in this Standard. For dated references, the subsequent
amendments (excluding corrigendum) or revisions do not apply to this Standard,
however, parties who reach an agreement based on this Standard are
encouraged to study if the latest versions of these documents are applicable.
For undated references, the latest edition of the referenced document applies.
GB 13917.1~13917.7, Laboratory efficacy test methods and criterions of
public health insecticides for pesticide registration
GB/T 17322.1~17322.11, Laboratory efficacy criterions of public health
insecticides for pesticide registration
Order of the General Administration of Quality Supervision, Inspection and
Quarantine (No.75) - “Measures for the Metrological Supervision and
Administration of Quantitatively Packed Commodities”
Order of the Ministry of Agriculture and Rural Affairs of the People’s Republic
of China [2007] (No.10) - “Pesticide registration information requirements”
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1 active ingredient
Chemical composition with biological insecticidal activity.
3.2 efficacy
Under the specified conditions and within the specified time, the effect of
repelling (killing) mosquitoes (including flies, cockroaches, ants and so on) the
product shall achieve.
3.3 median knockdown time, KT50
Under the specified conditions, the time required for 50% of the test insects to
be knocked down (i.e., fall down).
3.4 minimum effective period
The minimum effective time for the use of the traditional Chinese medicine liquid
of electrothermal mosquito liquid incense and electric heater.
4 Requirements
4.1 Requirements for use of active ingredient
It shall be the medicament that is registered for use in accordance with relevant
national regulations.
4.2 Toxicology
It shall meet the toxicological test requirements of the corresponding dosage
form in the Order of the Ministry of Agriculture and Rural Affairs of the People’s
Republic of China [2007] (No.10).
4.3 Active ingredient content and allowable fluctuation range
4.3.1 The content of active ingredients shall be clearly stated on the product
packaging.
4.3.2 The allowable fluctuation range of active ingredient content is shown in
Table 1 and the following regulations:
a) For mosquito coil, cockroach, fly incense and other tobacco preparation
products, the allowable fluctuation range of its active ingredient content
shall not be higher than 40% of the indicated value and not lower than 20%
of the indicated value;
b) For electrothermal mosquito liquid incense, the allowable fluctuation range
of its active ingredient content shall not be higher than 25% of the
indicated value and not lower than 10% of the indicated value;
c) Electrothermal mosquito tablet incense shall be marked (mg/piece). The
5.3 Active ingredient content and allowable fluctuation range
5.3.1 Visual inspection.
5.3.2 The content of active ingredients shall be tested in accordance with the
provisions of Annex A, Annex B, Annex C, and Annex D (unlisted dosage form
products shall be implemented according to the test methods in relevant
national standards).
5.4 Efficacy
5.4.1 Sprays, aerosols, small aerosols, mosquito coils, electrothermal mosquito
tablet incenses, electrothermal mosquito liquid incenses, cockroach poison
baits shall be tested according to GB 13917.1 ~ 13917.7.
5.4.2 Toxic powder, poison pen and repellent are tested according to GB/T
17322.9 ~ 17322.10.
5.4.3 Unlisted dosage form products are implemented according to the methods
in relevant national product standards.
5.5 Thermal storage stability
5.5.1 Mosquito coil
Take one coil from the middle of one box of test samples to crush. Pass the
0.154mm (100 mesh/inch) standard sample sieve. Take half of it and seal it in
a Teflon reagent bottle (the other half is tested for active ingredient content).
Then place it in a thermostat at (54±2)°C for 14d. After taking out the sample,
test and calculate the degradation rate according to the method for determining
the content of active ingredient within 24h.
5.5.2 Electrothermal mosquito tablet incense
The test sample shall be the electrothermal mosquito tablet incense in the same
row as before storage. The test sample (with aluminum foil packaging) is placed
in a (54±2)°C thermostatic chamber for 14d. After taking out the sample, test
and calculate the degradation rate according to the method for determining the
content of active ingredient within 24h.
5.5.3 Electrothermal mosquito liquid incense
Take a part of a bottle of test sample as the active ingredient content. Screw
the outer cover of the rest part into the original packaging. Then place in a
(54±2)°C thermostatic chamber for 14d. After taking out the sample, test and
calculate the degradation rate according to the method for determining the
content of active ingredient within 24h.
Liquid medicine is poured into a measuring cylinder or weighed with a balance.
Read out the test value (measuring cylinder division value: 0.1mL; balance
division value: 0.1g).
5.9 Internal pressure of insecticide aerosol
5.9.1 Instruments
5.9.1.1 Pressure gauge: range is 0~1.6MPa, accuracy is level 2.5.
5.9.1.2 Special joint.
5.9.1.3 Timer.
5.9.1.4 Constant temperature water bath: temperature control accuracy is ±2°C.
5.9.2 Test steps
Correctly press the valve actuator according to product description
requirements. Eliminate the air trapped in valves and straws. Then place the
sample in a (55±2)°C water bath. Immerse the water to four-fifths of the height
of the tank. Maintain it at the constant temperature for 30min. Wear thick leather
gloves. Remove the sample and dry it quickly. Unplug the valve actuator. Align
the pressure gauge inlet with the valve stem. Press hard. After the pressure
gauge pointer stabilizes, write down the pressure gauge reading. The maximum
value of three measurements shall prevail.
5.10 Net content of insecticide aerosol
5.10.1 Net volume of insecticide aerosol
5.10.1.1 Instruments
5.10.1.1.1 Glass aerosol test tube with scale: capacity is 90mL, minimum
division value is 1mL.
5.10.1.1.2 Balance: division value is not less than 0.01g.
5.10.1.2 Test temperature
The test temperature is (25±3)°C.
5.10.1.3 Test steps
Take the sample and weigh its mass m3. Assemble the glass aerosol test tube.
Use a valve without a straw. Wipe the glass aerosol test tube clean. First inject
a proper amount of propellant, about 10mL. Then spray empty and weigh its
mass m4.
Annex A
(normative)
Method for determining content of active ingredients in mosquito coils
A.1 Identification test
This identification test can be carried out simultaneously with the determination
of the content of active ingredients. Under the same chromatographic operating
conditions, the relative difference between the retention time of a
chromatographic peak in the sample solution and the retention time of the active
ingredient in the standard shall be within 1.5%.
A.2 Method summary
The sample uses dibutyl phthalate or dipentyl phthalate as the internal standard.
Conduct gas chromatography separation and determination on internal coated
SE-54 capillary column.
A.2.1 Instruments
A.2.1.1 Gas chromatograph: with hydrogen flame ionization detector.
A.2.1.2 Chromatography column: Φ0.25mm × 30m × 0.25μm, capillary column
coated with SE-54.
A.2.1.3 Micro syringe: 10μL.
A.2.1.4 Ground-mouth triangular flask.
A.2.1.5 Balance: division value is 0.1mg.
A.2.1.6 Grinder.
A.2.1.7 Sieve: standard sample sieve 0.154mm (100 mesh/inch).
A.2.1.8 Filter paper.
A.2.1.9 Oscillator.
A.2.2 Reagents
A.2.2.1 Internal standard substance: dibutyl phthalate or dipentyl phthalate,
without interference impurities.
A.2.2.2 Solvents: acetone, methanol (analytical reagent).
Annex B
(normative)
Method for determining content of active ingredients in electrothermal
mosquito tablet incense
B.1 Identification test
This identification test can be carried out simultaneously with the determination
of the content of active ingredients. Under the same chromatographic operating
conditions, the relative difference between the retention time of a
chromatographic peak in the sample solution and the retention time of the active
ingredient in the standard solution shall be within 1.5%.
B.2 Method summary
The sample uses dibutyl phthalate or diisooctyl phthalate as the internal
standard substance. Conduct gas chromatography separation and
determination on internal coated SE-54 capillary column.
B.2.1 Instruments
B.2.1.1 Gas chromatograph: with hydrogen flame ionization detector.
B.2.1.2 Chromatography column: Φ0.25mm × 30m × 0.25μm, capillary column
coated with SE-54.
B.2.1.3 Micro syringe: 10μL.
B.2.1.4 Ground-mouth test tube.
B.2.1.5 Ground-mouth triangular flask.
B.2.1.6 Balance: division value is 0.1mg.
B.2.2 Reagents
B.2.2.1 Internal standard substance: dibutyl phthalate or diisooctyl phthalate,
without interference impurities.
B.2.2.2 Solvents: acetone, methanol (analytical reagent).
B.2.2.3 Standard samples: allethrin, propargyl, etc.
B.2.3 Gas chromatography conditions
Annex C
(normative)
Method for determining content of active ingredients in electrothermal
mosquito liquid incense
C.1 Identification test
This identification test can be carried out simultaneously with the determination
of the content of active ingredients. Under the same chromatographic operating
conditions, the relative difference between the retention time of a
chromatographic peak in the sample solution and the retention time of the active
ingredient in the standard solution shall be within 1.5%.
C.2 Method summary
The sample uses dibutyl phthalate as the internal standard substance. Conduct
gas chromatography separation and determination on internal coated SE-54
capillary column.
C.2.1 Instruments
C.2.1.1 Gas chromatograph: with hydrogen flame ionization detector.
C.2.1.2 Chromatography column: Φ0.25mm × 30m × 0.25μm, capillary column
coated with SE-54.
C.2.1.3 Micro syringe: 10μL.
C.2.1.4 Ground-mouth test tube.
C.2.1.5 Ground-mouth triangular flask.
C.2.1.6 Balance: division value is 0.1mg.
C.2.1.7 Dropper with rubber head.
C.2.2 Reagents
C.2.2.1 Internal standard substance: dibutyl phthalate, free of interfering
impurities.
C.2.2.2 Solvents: acetone, methanol (analytical reagent).
C.2.2.3 Standard samples: allethrin, propargyrin, etc.
C.2.3 Gas chromatography conditions
C.2.3.1 Temperature
C.2.3.1.1 Column temperature: 220°C.
C.2.3.1.2 Gasification temperature: 250°C.
C.2.3.1.3 Detector temperature: 250°C.
C.2.3.2 Carrier gas: nitrogen.
The above operating conditions are typical operating parameters. According to
the characteristics of different instruments, the given operating conditions can
be adjusted appropriately in order to obtain the best results.
C.3 Preparation of standard solution
In a ground-mouth test tube, accurately weigh 0.03g~0.04g (to the nearest of
0.0002g) of standard sample equivalent to the sample to be tested. Then weigh
0.015g~0.025g (to the nearest of 0.0002g) of dibutyl phthalate. Add methanol-
acetone mixed solution. After fully dissolved, stopper and shake well, put in the
refrigerator for use.
C.4 Preparation of sample solution
In a ground-mouth test tube, accurately weigh 1g~4g (to the nearest of 0.0002g,
the ingredient to be tested is estimated about 0.03g~0.04g) of electrothermal
mosquito liquid incense to be analyzed. Then weigh 0.015g~0.025g (to the
nearest of 0.0002g) of dibutyl phthalate. Stopper and shake well, to be analyzed.
C.5 Determination
Under chromatographic conditions in C.2.3, after the instrument is stable, use
a micro syringe to continuously inject standard sample solution until the peak
area ratio of two adjacent needles and internal standard changes less than
1.5%. Conduct sample injection analysis in the order of standard sample
solution, sample solution, sample solution, and standard sample solution.
C.6 Calculation
Respectively average the ratio of the peak area of the sample peak to the
internal standard in the measured sample solution and the area ratio of the peak
of the two internal standards to the peak of the standard sample. According to
formula (C.1) and formula (C.2), calculate the mass fraction of the active
ingredient to be measured, Mx.
Correction factor:
D.2.3 Gas chromatography conditions
D.2.3.1 Temperature: the initial temperature of the column temperature is 220°C,
the retention time is 13min; the termination temperature is 260°C, the retention
time is 20 min; the heating rate is 20°C/min.
Gasification temperature: 270°C.
Detector temperature: 270°C.
D.2.3.2 Carrier gas: nitrogen.
The above operating conditions are typical operating parameters. According to
the characteristics of different instruments, the given operating conditions can
be adjusted appropriately in order to obtain the best results.
D.3 Preparation of internal standard solution
In a 100mL volumetric flask, weigh 0.3g~0.5g (to the nearest of 0.0002g) of
corresponding internal standard substance. Use acetone or absolute ethanol to
dissolve and set volume to scale. Shake well for use.
D.4 Preparation of standard solution
In a 50mL volumetric flask, accurately weigh various standard samples of an
amount equivalent to the sample to be tested, m1 (to the nearest of 0.0002g).
Add 5mL of internal standard solution. Set volume after complete dilution.
Stopper and shake well. Put in the refrigerator to use.
Method One:
D.5 Preparation of sample solution
In a clean 50mL volumetric flask, add 10mL of acetone or absolute ethanol.
Shake the entire bottle of aerosol. Pre-spray several times. Use a sprinkler with
a catheter (the end of the catheter is immersed in acetone or absolute ethanol)
and slowly spray about 10g of the drug solution (the mass m2 is obtained by the
weight reduction method, to the nearest of 0.001g). It can be placed in a 55°C
water bath. After slowly removing the propellant (until there are no obvious
bubbles), after adding 5mL of internal standard solution, use acetone or
absolute ethanol to set volume to the scale. Shake well for use.
D.6 Determination
Under chromatographic conditions in D.2.3, after the instrument is stable, use
a micro syringe to continuously inject standard sample solution until the peak
area ratio of two adjacent needles and internal standard changes less than
D.8 Preparation of standard solution
In a ground-mouth test tube, accurately weigh various standard samples of an
amount equivalent to the sample to be tested (to the nearest of 0.0002g). Then
weigh 0.015g~0.025g (to the nearest of 0.0002g) of dipentyl phthalate. Add 5mL
of acetone solution. After complete dilution, stopper and shake well. Put in the
refrigerator to use.
D.9 Sample pre-processing
Take a can of aerosol sample. Place it in a low temperature box at about -15°C
for 4h and take it out. Open a small hole with a diameter of about 0.2mm at the
top of the tank. Place in 46°C water bath for 1h. Let the propellant slowly
evaporate. Enlarge the hole. Pour out the liquid.
D.10 Preparation of sample solution
In a ground-mouth test tube, accurately weigh 10g of aerosol feed (to the
nearest of 0.0002g, depending on the amount of substance to be tested). Then
weigh 0.015g~0.025g of dipentyl phthalate. Stopper and shake well, to be
analyzed.
D.11 Determination
Under chromatographic conditions in D.2.3, after the instrument is stable, use
a micro syringe to continuously inject standard sample solution until the peak
area ratio of two adjacent needles and internal standard changes less than
1.5%. Conduct sample injection analysis in the order of standard sample
solution, sample solution, sample solution, and standard sample solution.
D.12 Calculation
Respectively average the ratio of the peak area of the sample peak to the
internal standard in the measured sample solution and the area ratio of the peak
of the two internal standards to the peak of the standard sample. According to
formula (D.3), formula (D.4) and formula (D.5), calculate the mass fraction of
the component to be tested, Mx.
Correction factor:
Mass fraction of ingredient to be tested:
cstandard
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.