This standard specifies the definition, technical requirements, test methods, inspection rules and marking, packaging, transportation, storage and instructions for use of electric heating sheet mosquito coils for household hygienic insecticides. This standard applies to tablets made of absorbable materials as carriers and added with insecticide liquid for repelling (killing) mosquitoes, which are used in conjunction with constant temperature electric heaters. At the rated heating temperature, the agent acts on mosquitoes in a gaseous state to achieve the effect of repelling (killing) mosquitoes. GB 18417-2001 Electric heating sheet mosquito coils for household hygienic insecticides GB18417-2001 Standard download decompression password: www.bzxz.net

GB18417—2001
Technical requirements 4.1, 4.4, 4.5.4.6 of this standard are mandatory, and the rest are recommended. Electric heating sheet mosquito coils for household hygienic insecticides are made of absorbent materials as carriers and insecticide liquids as tablets for repelling (killing) mosquitoes. They are used in conjunction with constant temperature electric heaters. At the rated heating temperature, the agent acts on mosquitoes in a gaseous state, achieving the effect of repelling (killing) mosquitoes. This standard is formulated on the basis of the original light industry standard QB1692.21993 of the People's Republic of China "Electric heating sheet mosquito coils for household hygienic insecticides", and the contents of each chapter are appropriately modified and supplemented to make the standard more standardized and the content more constitutional. At the same time, the appendix A and appendix B of the standard explain in detail the determination method of effective ingredients, which is applicable to the test needs of different columns of gas chromatograph capillary column and packed column; the indoor efficacy determination method of electric heating sheet mosquito coil Appendix C quoted GB 13917.5-1992 "Indoor efficacy test method of pesticide registration and sanitary insecticide indoor efficacy determination method of electric heating sheet mosquito coil", and redefined the indoor temperature of the test room in combination with the actual situation.
From the date of implementation, this standard will replace QB1692.2-1993. The appendix A, appendix B and appendix C of this standard are all appendices of the standard. This standard is proposed by China Light Industry Federation. This standard is under the jurisdiction of the National Daily Miscellaneous Products Standardization Center. The drafting units of this standard are Shanghai Johnson Co., Ltd., Guangdong Zhongshan Gaiju Yue Products Co., Ltd., Guangxi Liuzhou Huali Household Products Co., Ltd.
The main drafters of this standard are Hu Xuedun, Lin Wei, Zhou Jilan, and Yang Laimei. 711
1 Scope
National Standard of the People's Republic of China
Household sanitary insecticide
Electrothermal mosquito tablet incense:
Domestic sanitary insecticideElectrothermal mosquito tablet incenseGB 18417—2001
This standard specifies the definition, technical requirements, test methods, inspection rules and marking, packaging, transportation, storage and instructions for use of household sanitary insecticideElectrothermal mosquito tablet incense.
This standard applies to tablets made of absorbable materials as carriers and added with insecticide liquid for repelling (killing) mosquitoes, which are used in conjunction with constant temperature electric heaters. At the rated heating temperature, the agent acts on mosquitoes in a gaseous state to achieve the effect of repelling (killing) mosquitoes. 2 Referenced Standards
The provisions contained in the following standards are constituted as provisions of this standard through reference in this standard. When this standard was published, the versions shown were all valid. All standards are subject to revision. Parties using this standard should explore the possibility of using the latest versions of the following standards. GB/T 2828-1987
GB/T2829—1987
GB5296.1--1997
Counting sampling procedures and sampling tables for batch inspection (applicable to inspection of continuous batches)Counting sampling procedures and sampling tables for periodic inspection (applicable to inspection of production process stability)General instructions for consumer products
GB13917.5—1992
Pesticide registrationIndoor efficacy test method for hygienic insecticidesIndoor efficacy determination method for electric heating sheet mosquito coils
3 Definitions
This standard adopts the following definitions.
3.1 Knockdown time (KT50 value)
The time required for 50% of the test insects to be knocked down (i.e., lying on their backs) under specified conditions. 3.2 Efficacy
The product should achieve the effect of repelling (killing) mosquitoes under the specified conditions and within the specified time. 3.3 Active ingredients
Chemical ingredients with biological insecticide activity. 3.4 Test angle
A device that can make the tested sample in a place without the influence of external airflow. 4 Technical requirements
4. 1 Medication requirements
Must be a drug registered or approved for use by relevant national government departments. 4.2 The dimensions of mosquito coils shall comply with the provisions of Table 1. Approved by the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China on August 28, 2001, 702-iiKAONiKAca-
Implemented on July 1, 2002
4.3 Appearance and sensory experience
4.3.1 Appearance
GB 18417-200T
Electric thermometer mosquito coils shall have an indicating color, which shall be uniform and shall not change. 4.3.2 Sensory experience
No irritating odor.
4.4 Active ingredient content
The active ingredient content of the product must be clearly indicated on the packaging, and the relative deviation of the active ingredient content is 1%. 4.5 Thermal storage stability
After the thermal storage stability test, the degradation rate of the active ingredient content of pyrethroids is 5%, and the degradation rate of the active ingredient content of other types is 10%. 4.6 Drug efficacy
Cylinder method KT50≤5min or box method KT507min5 Test method
5.1 Drug requirements
Check whether there is a registration or identification certificate for the drug5.2 External dimensions
Measure with a caliper (accuracy 0.02 mm).
5.3 Appearance and sensory perception
Use the day measurement method and the membrane perception method, and check under normal light at a distance of 250mm from the sample to be tested. 5.4 Pharmaceutical
5.4.1 Active ingredient content
The determination method is shown in Appendix A and Appendix B, of which Appendix A is the arbitration method; for products to which the active ingredient analysis method of this standard is not applicable, the manufacturer shall provide the analysis method.
5.4.2 Thermal storage stability
Put the test sample (with aluminum foil packaging) in a constant temperature box at (54-2) for 14 days: after taking it out, measure its degradation rate according to the method of active ingredient content.
5.4.3 Degradation rate
The degradation rate is calculated according to formula (1):
4(%)=Zi\yi×100
Wherein, degradation rate
m is the active ingredient content of the sample measured before thermal storage; m is the active ingredient content of the sample measured after thermal storage. See Appendix C for the determination method.
6 Inspection rules
6.1 Products must be inspected and qualified by the quality inspection department of the manufacturer according to this standard before they can be shipped, and instructions for use and inspection certificates are attached. 6.2 Inspection is divided into delivery inspection and type inspection. 703
6.2.1 Factory inspection
GB 18417—2001
All products proposed for delivery shall be subject to factory inspection. Factory inspection adopts the normal inspection and sampling plan of GI3/T2828 special inspection level S-2. The inspection items and qualified quality level AQ1. values ​​are shown in Table 2. Table 2
6.2.2 Type inspection
Inspection items
Dimensions
Appearance and sensory
Technical requirements clauses
6.2.2.1 Type inspection shall be carried out in any of the following cases. a) Trial production and identification of new products and old products for transfer to factory production: test method clause
h) After formal production, if there are major changes in structure, materials, and processes that may affect product performance, c) During normal production, sample and check batch products at least once a year; d) When the product is discontinued for more than half a year and resumed; e) When the factory inspection results are significantly different from the 1st type inspection: 1) When the national quality supervision and inspection agency proposes a type inspection requirement. AQL
6.2.2.2 Type inspection uses the GR/T2829 discrimination level I sampling plan, and its inspection items, unqualified quality level RQL value, accompanying size and judgment array are shown in Table 3. If one item is unqualified in the type inspection, it will be comprehensively judged as unqualified. Table 3
Inspection items
H
Dimensions
Appearance and feel
Hot storage stability
Content of active ingredients,
Marking, packaging, transportation, storage, instructions for use 7.1 Marking
7.1.1. The product packaging box L should have the following Chinese content: a) Product name, trademark, factory name, address: b) Active ingredients and content:
c) Product standard number;
Sample size
Determination array
No drug registration or adjustment certificate, judged as unqualified 5
Degradation rate
Pyrethroids>5% is judged as unqualified
Others ≥10% is judged as unqualified
Simple method KT505min is judged as unqualified
Square box method KT50>7 min is judged as unqualified Exceeding the value indicated on the package + 10% is judged as unqualified d) Production and shelf life or production batch order and expiration date, e) Product quality inspection certificate:
f) Specifications and quantity
7.1.2 The product packaging box should have the following Chinese content: a) Pictorial logo;
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b) Product name and specifications:
e) Quantity;
d) Gross weight (kg),
GB18417-2001
e) Production date and shelf life, production batch number and expiration date; f) Manufacturer's name and address
g) Overall dimensions: length x width x height (cm). 7.2 Packaging
The product should be sealed with moisture-proof, light-proof and airtight packaging materials (such as aluminum foil composite packaging bags). The packaging must be firm, undamaged, moisture-proof and dew-proof.
7.3 Transportation
The product should be handled with care to prevent severe vibration, traffic, rain and heavy pressure. 7.4 Storage
The product should be stored in a cool, dry and ventilated warehouse and should not be mixed with flammable or explosive items. Under the above conditions, the shelf life of the product is not less than two years.
7.5 Instructions
The instructions for use of the product should comply with the provisions of GB5296.1. 705
A1 Identification test
GB 18417—2001
Appendix A
(Appendix of the standard)
Determination method of effective ingredients in electric heating sheet mosquito coils (I) This identification test can be carried out simultaneously with the determination of the content of the common name of the effective ingredient. Under the same chromatographic operating conditions, the relative difference between the retention time of the sample solution base "chromatographic peak" and the retention time of the standard solution (common name of the active ingredient) should be within 1% 5%. A2 Method Summary
The sample uses dibutyl phthalate or diisooctyl phthalate as the internal standard, and is separated and determined by gas chromatography on an internally coated SE-54 capillary column.
A2.1 Instrument
A2.1.1 Gas chromatograph: with hydrogen flame ionization detector. A2.1.2 Chromatographic support: $0.25mm×30m internally coated $E54 capillary column. A2.1.3 Micro syringe: 10 μL,
A2. 1. 4 Weighing bottle: 15 ml.
A2. 1. 5 Grinding stopper test tube: 25 mL.
A2.1.6 Balance: Graduation value is 0.1mg.
A2.2 Reagents
A2.2.1 Internal standard: monobutyl phthalate, diisooctanol phthalate, without interfering impurities (scope of application of internal standard: dibutyl phthalate is applicable to samples without oxidized piperonyl butoxide, i.e. S, and diisooctanol phthalate is applicable to samples with oxidized piperonyl butoxide),
A2.2.2 Solvent: acetone, methanol (analytical grade). A2.2.3 Standards: allethrin, propylthrin, etc. A2.3 Gas chromatography conditions
A2.3.1 Temperature
A2.3.1.1 Column temperature: 220°C or 260°C. A2.3.1.2 Vaporization temperature: 250°C or 270°C. A2.3.1.3 Detector temperature: 250°C or 270°C. A2.3.2 Gas flow rate (kg/m\).
A2.3.2.1 Carrier gas: Nitrogen 1.0, A2.3.2.2 Fuel gas: Hydrogen 0. 6. A2.3.2.3 Combustion-supporting air 0.5,
1 The above operating conditions are typical operating parameters. According to the characteristics of different instruments, the given operating conditions can be appropriately adjusted in order to obtain the best results.
A3 Preparation of standard solution
Accurately weigh the standard sample and internal standard in a 15mL weighing bottle (see Table A1 for the sample weight), add 5mL of acetone solution, and after fully dissolving, seal the bottle and put it in the refrigerator for use. 706
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Internal standard
Weigh the sample
Butyl phthalate
Di-2-ethylhexyl phthalate
A4 Preparation of sample solution
A4.1 Pretreatment of samples
GB 18417—2001
Weighing sample ratio
Standard sample: internal standard -1.5~2.0:1
Standard sample: internal standard = 1:1.2~1.5
Take a piece of electric heating plate mosquito coil finished product, cut it into strips with scissors and peel it off for use. A4.2 Preparation of electric heating plate mosquito coil extract
Weigh sample mother (fine to (.1012 g)
Standard sample 0.03g-0.04K
Internal standard 0.015g.C20g
Standard sample 9. 02g~0. 03g
Internal standard 0. 03 g~0. 04 g
In a 25 mJ ground-mouth test tube, weigh 0. 015 dibutyl phthalate. 0.020 g or 0.03g~0.04g of diisophthalic acid (depending on the amount of the component to be tested), put the treated electric heating mosquito coil into a test tube, add 10mL of methanol acetone mixed solution (volume ratio 1:1), it is appropriate to submerge the tablets, shake them fully, soak them for 1h, shake them vigorously before analysis, and take the upper clear liquid for analysis.
A5 Determination
After the instrument is stable under the chromatographic conditions of A2.3, continuously inject the standard solution and sample solution with a micro syringe, calculate the peak area ratio of the sample (standard sample) to the internal standard in the chromatogram of each needle, and wait until the peak area ratio of the two adjacent needles is basically parallel and stable. Perform gas chromatography analysis according to the above conditions.
A6 Calculation
Average the measured area ratios of the sample peaks to the internal standard peaks in the two sample solutions and the area ratios of the two internal standard peaks to the standard sample in the standard solution. Calculate the content Mx of the component to be measured according to formulas (A1) and (A2). Correction factor:
The content of the component to be measured;
Where: A.
f=A2Xmiz/ms2 XCstandard
Mx=fX A,Xmsl
The average value of the area ratios of the sample peaks to the internal standard peaks in the sample solution; AThe average value of the area ratios of the internal standard peaks to the standard sample peaks in the standard solution; m: the mass of the internal standard in the sample solution, g: m2, the mass limit of the internal standard in the standard solution; Certificate 2—the mass of the standard substance in the standard solution; Cstandard—the content of the standard substance, which is.
Appendix B
(Standard Appendix)
Determination Method of Effective Ingredients in Mosquito Repellent Coils (II) B1 Identification Test
This identification test can be carried out simultaneously with the determination of effective or common name content. Under the chromatographic operating conditions of the sample solution, the retention time of a certain color peak and the retention time of the standard solution (common name of active ingredient) should be within 1 to 5 seconds. B2 Method Summary
The sample is separated and determined by gas chromatography on a 5% SE-30 packed column with dibutyl phthalate as the internal standard. B2.1 Instrument
B2.1.1 Gas chromatograph: with a hydrogen flame ionization detector. B2.1.2 Chromatographic properties: 3 1-1In×2 tm, glass column or stainless steel column filled with 5% SE-30 coated on Chromel AWDmcs 8~100 mesh chromatographic support.
B2.1.3 Micro syringe: i0 μL
B2.1.4 Weighing bottle: 15 ml..
Grinding stopper test tube; 25 mL.,
#2.1.6 Balance: Graduation value is 0.1mg:
B2.2 Reagents
B2.2.1 Internal standard: o-butylaldehyde of dimethic acid - without -7 interfering impurities. B2.2.2 Quenching agent: acetone, medium alcohol (analytical grade). B2.2, 3 Standard filling products: allethrin, propylthrin, etc. B2.3 Gas chromatography conditions
B2.3.1 Temperature
B2.3. 1. 1 Column temperature: 180°C
B2.3.1.2 Degree of chromatographic concentration: 250°C.
H2.3.1.3 Detector temperature: 250C.
B2.3. 2 Gas flow rate (kg/cim).
B2.3. 2.1 Carrier gas: nitrogen 1.0.
B2.3.2.2 Fuel gas: hydrogen 0.6
B2.3.2.3 Fuel gas: air 0.6. bzxZ.net
The above operation cases are typical operation parameters. According to the characteristics of different instruments, the given operation conditions can be appropriately adjusted to obtain the best effect.
B3 Preparation of standard solution
Accurately weigh the sample and internal standard in a 15 ml weighing bottle (see Table B1 for the sample weight), add 5 mL of acetone solution to fully dissolve, seal and mix well, and put in the refrigerator for use. Table B1
Internal standard
Weighing amount
Diisopropyl acetate
B4 Preparation of sample solution
B4. 1 Pretreatment of sample
Weighing sample Ratio
Standard sample: internal standard = 2~2.5: 1
Cut a piece of electric heating sheet into strips with scissors and peel it off for standby use. B4.2 Preparation of mosquito coil extract
Sample amount (sugar to 0.0002 g)
Standard sample 0.0300g~0.0450g
Internal standard 0.0150~0.0200 g
Accurately weigh 0.015g~0.020g (depending on the concentration of the component to be tested) of dibutyl ketone of phthalate in a 25 mL test tube (708
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GB 18417—2001
Put the treated mosquito coil in a test tube, add methanol-ketone mixed solution (volume ratio]: 1) 1 mL, enough to submerge the tablets. Shake thoroughly and soak for 1 h. Shake vigorously again before analysis, and take the upper clear liquid for analysis. B5 Determination
Under the chromatographic conditions of B2.3, after the instrument is stable, inject the standard solution and sample solution continuously with a micro-syringe, calculate the peak area ratio of the sample (standard sample) to the internal standard in each needle chromatogram, wait until the peak area ratio of the two adjacent needles is basically parallel and stable, and perform gas chromatography analysis under the above conditions.
B6 Calculation
Average the measured sample peak to internal standard peak area ratios in the two sample solutions and the two internal standard peaks to standard peak area ratios in the standard solution, and calculate the content Mx of the component to be measured according to formula (BI) and formula (B2). Calibration factor:
The content of the component to be tested:
Wu Zhong: A,
f=AXmi/mXCt
M-JXA× m1
The average value of the area ratio of the sample peak to the internal standard peak in the sample solution: The average value of the area ratio of the internal standard peak to the standard peak in the standard solution: The mass of the internal standard in the sample solution -&!
The mass of the internal standard in the standard solution, g; -The mass of the standard substance in the standard solution·g: The content of the standard substance,
Appendix C
(Standard Appendix)
Method for determining the indoor efficacy of electric heating mosquito coils
C1 Test insects: Standard test insects are used
Mosquito: The beach adult mosquito that has not sucked blood on the 2nd to 3rd day after emergence. In the northern region, Culex pipiens is used, and in the southern region, Culex pipiens is used. C2 Test system
Room temperature: (26=2)℃
Relative filtration: (605)
C3 Instrument
C3. 1 Closed cylinder device (Figure C1): A glass or transparent colorless plastic cylinder (C) with an inner diameter of 2cm and a height of 13cm is placed on the frame (I). I: There are two glass or transparent colorless plastic plates (E, F) with a diameter of 27cm on the upper and lower sides of the cylinder. The upper plate has a hole with a diameter of 2cm in the center, which is plugged with a rubber plug (C). There is a hole with a diameter of 5cm in the center of the lower plate. During the fumigation treatment, the electric mosquito coil blood heater is placed under the hole. Before and after the fumigation treatment, the hole is plugged with an amine plug (H). The joints between the round cylinder and the upper and lower plates are respectively cushioned with rubber washers (DI, I) to prevent the leakage of the agent. C3.2 Glass box device (Figure C2): Glass square box, placed on an aluminum frame, length, width and height are 70cm. There is a small door with a width and height of 0.2 at the lower corner of the side. There is a discharge hole on the upper side of this side, which can be plugged with a rubber plug. There is another side and the whole is a big door. A uniform layer of self-paint is applied to the outer surface of the bottom of the box. During the test, the whole device is sealed with a case seal. C3.3 Electric heating plate mosquito coil heater: working voltage 229 V, working temperature (165 5) C. C3.4 Mosquito suction tube,
C3.5 Stopwatch.
C3.6 Counter.
C4 Test steps
Dai steam towel
GH 18417—2001
Figure C1 Closed toilet device
After fumigation
A--Incandescent mosquito coil dye sheet; B--Electric mosquito coil device; C--Glass or transparent colorless plastic mesh tube, height 13cm, inner diameter 1mm; D--Rubber ring; F--Glass or transparent colorless plastic round plate, diameter 27cm, with a round hole of 2rm in the center; G, H..Rubber plug; T--Stand, height 30cm]--12-sieve moon-shaped wire mesh
Figure C2 Glass box device
L--Glass square box, length, width and height are all 70 cm1; C--Small door, width and height are all 10 cm; D--door, E--aluminum frame: F--insect hole. Diameter 5 cm--tighten with rubber plug C4.1 Steps for efficacy determination using closed circular device The electric heating sheet mosquito coil sample should be tested after preheating for 1 h, 2 h, 4 h, 6 h, 8 h (if the efficacy of the product exceeds 8 h, the time indicated should also be followed).
Use a mosquito suction tube to suck 20 test mosquitoes from the breeding cage and insert them from the central circular hole of the circular plate (F) below the closed circular device, and plug the rubber plug 710
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GB18417—2001
(H): When the test insects resume normal activities, place an electric heating sheet mosquito coil heater under the central circular hole of the lower test plate (F), and place a wire mesh above it: to prevent the knocked-down test mosquitoes from falling on the electric heating sheet mosquito coil heater. The electric heating sheet mosquito coil heater must be fastened to the middle fire round hole of the lower round plate (F) and accurately black kill! min, while timing. After fumigation, cut off the power supply, remove the electric heating sheet mosquito coil heater and the electric heating sheet mosquito coil sample, immediately plug the rubber plug (H), and record the number of test mosquitoes knocked down at regular intervals. The test has at least three repetitions, and at least 15 tests should be performed. After each test, the entire test device must be cleaned before the next test. At the same time, a blank test must be performed immediately. If the knockdown rate and mortality rate of the blank test are greater than 20, the entire test must be repeated. C4.2 Efficacy determination using glass box device Step The electric heating sheet mosquito coil sample should be tested after power on preheating for 1h.2h, 4h, 6h.8h (the product's stated efficacy exceeds 8h and should also be tested according to the stated time).
Use a suction tube to suck 40 test mosquitoes from the breeding cage and release them from the insect release port of the glass box device. When the test mosquitoes resume normal activity, put the preheated electric heating plate samples and electric heating plate mosquito-repellent incense heaters into the center of the glass box through the small door at the lower corner of one side of the glass box device, and place a wire mesh on the side to prevent the knocked-down test mosquitoes from falling on the electric heating plate mosquito-repellent incense heater. Immediately close the entire glass box device, seal it with a tape, start killing, and count the number of knocked-down test mosquitoes at regular intervals. The test must be repeated at least three times. In practice, at least 5 tests must be performed. After each test, the entire test device must be cleaned before the next test. A blank test must be performed on the opposite side. If the knock-down rate and mortality rate of the blank test are greater than 20, the test must be repeated. C5 calculation
The three repeated data of the test are connected to the value method to calculate K150. When the test results of the square box method and the circle method conflict, the test results of the square box method shall prevail. 711
GB 18417- -2001
GB184162001 Amendment No. 1 to 4 national standards including household hygienic insecticide coil mosquito coils
The amendment has been approved by the National Standardization Administration on February 10, 2003 with the document [2003] No. 9 of the National Standardization Administration, and will be implemented from the date of promulgation.
GB18417-2001 Household hygienic insecticide electric heating sheet mosquito coils" Article No.
6.2.2.2 Table 3
Hot storage stability
6,2.2.2 Table 3
The technical requirements of 4.1, 4.4.4.5 and 4.6 of this standard are mandatory. The rest are recommended.
.·, the machine deviation of the effective ingredient content is ±10%. , the degradation rate of the effective or sub-content of pyrethroids is 5%,The degradation rate of other active ingredients is 10%.
Modify to
4.1, 4.4, 4.5.4.6.7.1.1, 7.4 of this standard? And are mandatory, the rest are recommended, ..., the active ingredient content shall not be lower than the maximum content explicitly stated in the product,
, the degradation rate of pyrethroid active ingredients is
10%. The degradation rate of other active ingredients is less than 15%.
Circle method KT50≤5min or square box method KT50Circle method KT50≤8.0min or square box method? min.
5. 4. 1 Active ingredient content
5.4.2 Heat storage stability
=.4.3 Degradation rate
5.5 Efficacy
: Pyrethroids>5% are judged as unqualified
Others 10% are judged as unqualified
Reading tube method KT50>5min.
Square method KT 50 >7 min....
6.2.2.2 Table 3! Exceeding the value indicated on the package = 10 years old Active ingredient content
is judged as unqualified
(depending on the amount of the ingredient to be tested),
. (depending on the amount of the ingredient to be tested),
KT 50≤10 min
Active ingredient content
Remove 5.4.1 Active ingredient content\this title 5.5 Hot paste stability
5.5.1 Calculation of degradation rate
5.5 Efficacy
Pyrethroids 10 is judged as unqualified
Others 15% is judged as unqualified
Cylinder method KT 50~8.0 min**
Square box method KT 3 ≥l0.0 If the value is lower than the value indicated on the package, it is considered unqualified. (accurate to 0.0002g, depending on the amount of the component to be tested), (accurate to 0.0002g, depending on the amount of the component to be tested)
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