ICS 65.100.10 
G25 
GB 
 
National Standards of the People’s Republic of China 
         GB XXXX----XXXX 
 
  
 
 
d-allethrin technical material  
 
(Draft) 
     
Published XX – XX – XXXX                      Effective as of XX – XX – XXXX  
Issued by the 
General Administration of Quality Supervisi on, Inspection and Quarantine of the People's 
Republic of China (AQSIQ) and  
the Standardisation Administration of the People’s Republic of China (SAC)GB XXXXX – XXXX 
Foreword 
Chapter 3 and 5 of these standards are mandatory. The rest are recommendations.  
These standards are drafted in accordance w ith the rules stipulat ed in GB/T 1.1-2009. 
These standards are proposed by China Pe troleum and Chemical  Industry Federation 
(CPCIF). 
The compilation of these standards was manage d by the National Standa rdisation Technical 
Committee on Pesticides.   
These standards were drafted by Jiangsu Ya ngnong Chemical Co. Ltd with contributions by 
Aestar (Zhongshan) Co. Lt d and LIBY Group Co. Ltd.  
Main persons responsible for drafting these standards: Weirong Liu, Weilian Shi, Bin Lin, 
Shen Ruan and Zuoyi Yang. d-allethrin compound  
 
1. Scope of these standards 
These standards stipulate the requirements re lating to testing methods, marking, labelling, 
packaging, storing and transport for d-allethrin. 
These standards are used for d-allethrin wh ich consists of d-a llethrin with related 
manufacturing impurities. 
Note: Please refer to Appendix A for the structural formula, information and other names of d-allethrin.    
 
2.  Reference documents 
The following documents are essential to the ap plication of these standards. For reference 
documents which are dated, only the dated versio ns are applicable to these standards. For 
reference documents which are not dated, the la test versions (includi ng all amendments) are 
applicable to these standards.  
GB/T 601 Chemical reagent – preparations of standard volumetric solutions 
GB/T 1600 Testing method of water in pesticides GB/T 1604 Regulation concerning acceptanc e checks for commercial pesticides 
GB/T 1605-2001 Sampling method for commodity pesticides GB 3796 General rule for packing of pesticides 
GB/T 6682-2008 Water for analytical laborator y use – specification and test methods 
GB/T 8170-2008 Rules of rounding off for numerica l values & expression and judgement of 
limiting values 
 
3. Requirements 
3.1 Composition and appearance 
The material consists of d-allethrin with rela ted manufacturing impurities. It is a yellowish-
brown, oil-like liquid.  
3.2 d-allethrin should meet the requirements set out in Table 1. 
Table 1  d-allethrin, value of indicators 
Item Value 
Allethrin content / % ≥ 95.0 Dextrorotatory ratio / % ≥ 95.0 
Cis/trans isomerism of acid (20 ± 5) / (80 ± 5) 
Acidity (measured by H2SO4) / % ≤ 0.3 
Water content / % ≤ 0.3 
 
4. Testing methods 
4.1 General rules 
Unless otherwise stated, the reagent and wate r referred to in these standards are the 
analytical reagent (AR) and the third grade water described in GB/T 6682-2008. 
Unless otherwise stated, the standa rd volumetric solution used in this test should be prepared 
and calibrated in accordance with GB/T 601. All results should be rounded and analysed in 
accordance with 4.3.3 of GB/T 8170-2008. 
4.2  Sampling 
Sampling should be conducted in accordance wi th the method described under "sampling for 
commodity compound” in GB/T 1605 – 2001. The number of packages sampled should be 
determined by the “random rule” and the vol ume sampled should be no less than 100g.  
4.3 Tests 
Both tests below are valid. Either test can be  chosen to identify the compound. If it is not 
possible to produce a conclusive result with one test, the other test should also be conducted 
in order to confirm the result.     
Gas chromatography. This test can be carried out  together with the allethrin content test. 
Under the same conditions, the difference betw een the retention time peaks for the sample 
and the retention time peaks for the reference st andard (allethrin) should not exceed 1.5%.    
Infrared spectrometry. In the region of 4000 cm-1 ~ 400 cm-1, the absorption spectrums 
between the sample and the d-allethrin reference standard should be very similar. Please see 
graph 1 for the infrared spectrum of the d-allethrin reference standard. 
 
Graph 1 Infrared spectrum of d-allethrin reference standard 4.4 Allethrin content test 
4.4.1 Method 
Dissolve the sample in ethyl acetate; use dibutyl  phthalate as the internal standard; use a 30 
m x 0.32 mm HP-1 capillary column and flame ionization detector; separate and analyse the 
sample using gas chromatography.   
4.4.2 Reagents and solutions Allethrin reference standard: known allethrin content, ω ≥ 98.0%; 
Dibutyl phthalate; 
Ethyl acetate; 
Internal standard solutio n: dissolve 0.7 g of dibutyl phthalate  with ethyl acet ate in a 100 mL 
volumetric flask and shake well.  
4.4.3 Instruments 
Gas chromatograph: with flame ionization detector; 
Gas chromatograph data pro cessing machine or software; 
Column: 30 m x 0.32 mm (i.d.) quartz capi llary column, with HP-1 (100% 
dimethylpolysiloxane) applied to the inner wall at a thickness of 0.25 μm. 
4.4.4 Conditions 
Temperature (
℃): column 200, inlet 250, detector 250. 
Flow rate (mL/min): carrier gas (N 2) 1.6, hydrogen 30, atmosphere 400; 
Split rate: 30:1;  
Amount injected: 0.6 μL; 
Retention time (min): internal standard 2.9 approximately, allethrin 4.4 approximately; 
The above standard parameters can be adjusted when using different instruments in order to 
achieve the best results. Pleas e see graph 2 for the standard gas chromatograph spectrum of 
allethrin.  
 1 – Internal standard; 
2 – Allethrin. 
Graph 2   Gas chromatograph spectrum of allethrin compound and internal standard 
 
4.4.5 Steps 
4.4.5.1 Preparation of reference standard 
Add 0.10 ~ 0.12g (accurate to 0.0002 g)  of allethrin to a clean, dry 15 mL bottle (with a cap). 
Use a pipette to add 10 mL of intern al standard solution and shake well. 
4.4.5.2 Preparation of sample 
Add 0.10 ~ 0.12g of allethrin (accurate to 0.0002 g) to a clean, dry 15 mL bottle (with a cap). 
Use the same pipette as in 4.4.5.1 to add 10 mL of  internal standard so lution and shake well. 
4.4.5.3 Analysis 
Under the conditions specified a bove and when the instrument is stabilised, continuously 
inject the sample into the chromatograph. The analysis can be carried out when the 
difference in peak area ratio (allethrin: intern al standard) between tw o injections is below 
1.2%. The analysis should be conducted in the following order: reference standard, sample, 
sample and reference standard. 
4.4.6 Calculation 
Calculate the average the peak area ratio (allethr in: internal standard) of two injections of the 
sample; then calculate the average of two injec tions of reference standard before and after 
the injection of the sample; the allethrin conten t in the sample can then be calculated based 
on formula (1):  
 r2 × m1 × ω 
ω1 =  -------------------- …………...………..(1) 
 r1 × m2  
Where: 
ω1  =  Mass/presence of allethrin in sample (%) 
r2  = The average peak retention time of the allethrin sample and the internal standard. 
r1  = The average peak retention time of the refe rence standard and the internal standard. 
m1  =  The mass of allethrin in the reference sample (g) 
m2  = The mass of the allethrin test sample (g) 
ω  = The proportional content of allethri n in the reference standard (%) 
 
 4.4.7 Tolerance 
The parallel allethrin content readings should have a discrepancy of less than 1.2%. Take the 
calculated average as the final result. 
 
4.5 Dextro-isomer ratio and the determin ation of isomer and trans-isomer 
 composition 
4.5.1 Overview of the method   
After the sample has undergone saponifica tion and acidulation treat ment, separate and 
determine the acidified product using a β DEX-120 coated quartz capillary column, split 
injection device and flame ionization detector (FID). Then use this reading to calculate 
the amount of displaced chrysanthemic acid.  
 
4.5.2 Reagents and solutions 
Sodium hydroxide methanol solution:  ω (NaOH) =10% 
Hydrochloric acid: ω(HCI) =10% 
Diethyl ether  
4.5.3 Instruments 
Gas chromatograph (GC): with fl ame ionization detector (FID); 
Capillary column: 30 m × 0.25mm (i.d) fused s ilica column, with an internal coating of β 
DEX-120, to a thickness of 0.2µm; 
Sample injector apparatus: split silica lined   Conical flask: 100ml 
Separating funnel: 60ml 
Spherical condenser: 200mm 
 
4.5.4 Operating conditions 
Temp (ºC): Column 150; vaporising chamber 250; detection chamber 250;  
Gas flow volume (mL/min): carrier ga s (He) 1.6, Hydrogen 30, Atmosphere 400; 
Flow ratio: 30:1; Sample volume: 0.6 µL; Retention time (min): 1R, trans; 1R chrysa nthemic acid 9.2; 1R,cis; 1R chrysanthemic 
acid  9.5; 1R, trans; 1S chrysanthemic acid 9.7; 101R, cis; 1S ch rysanthemic acid 10.0; 
The above guidelines produce the standard refe rence results. Small adjustments can be 
made according to the specific requirements of certain instruments in order to achieve the 
most accurate results. Figure 3 shows a standard chromatograph for dextro-
chrysanthemic acid. 
 
 
1. + trans  chrysanthemic acid  
2. + cis chrysanthemic acid  
3. – trans  chrysanthemic acid      
4. + cis chrysanthemic acid  
 
Chart 3  Chromatograph for dextro-chrysanthemic acid 
 
4.5.5 Method for determination 
4.5.5.1 Preparing the sample solution 
Take approximately 0.4g of the sample and pla ce in a conical flask. Add 10ml of Sodium 
Hydroxide methanol solution (10% concentratio n) and place in a water-bath at 50-60ºC 
to saponify. Add a further 10ml of water and dissolve, then extrac t twice using diethyl 
ether. Use 10ml of diethyl each time. Extract the lower layer twice and then add together. 
Then add a solution of hydrochloric acid (con centration of 10%) to bring the water layer 
to pH3-4. At this point add a further 10ml of  diethyl ether and extr act once again before 
extracting the upper laye r of dextro-chrysanthemic acid which is now ready to use.  
4.5.5.2 Determination 
Set up the GC according to the directions abov e, wait for the instrument to stabilise and 
then add the sample solution. 
4.5.6 Calculations 
Dextro-isomer composition is calculated using the formula ώ2 (2): 
      A1+A 2 
     ω2 = --------------- ---------    × 100 ……………(2) 
     A1 + A 2 + A 3+ A 4  
Where: 
A1 = + trans  chrysanthemic acid peak retention; 
A2 =  + cis chrysanthemic acid peak retention; 
A3 =  – trans  chrysanthemic acid peak retention; 
A4 =  + cis chrysanthemic peak retention. 
 
4.5.7 Determination of acid cis-isom er and trans-isomer composition 
The determination of acid cis-isomer and tr ans-isomer composition a nd that of the acid 
1R isomer can be carried out at the same time. 
The composition of cis-isomers and trans- isomers can be calculated using formula a (3): 
 
     A 2+A 4 
    ___________________________ × 100  
        A 1 + A 2 + A 3+ A 4 
   a = __________________.................................................. (3) 
             A 1   + A 3 
    ___________________________ × 100  
      A 1 + A 2 + A 3+ A 4Where:  
A1 = + trans  chrysanthemic acid peak retention; 
A2 =  + cis chrysanthemic acid peak retention; 
A3 =  – trans  chrysanthemic acid peak retention; 
A4 =  + cis chrysanthemic peak retention. 
 
Determination of acidity levels 
4.6.1 Chemical reagent/solution  
Pure ethanol; 
Sodium hydroxide titrate so lution: c (NaOH) = 0.01 mol/L; 
Methyl red: 1g/L ethanol solution; Bromocresol green: 1g/L ethanol solution; Compound indicator: Mix together 2ml of methyl  red solution and 10ml of bromocresol 
green solution. 
4.6.2  Procedure  
Place 2g of a-allethrin (accura te to 0.0002g) in a 250ml laboratory beaker and add 50 ml 
of pure ethanol and shake until evenly dilute d; add 6 drops of co mpound indicator, and 
then add sodium hydroxide titrate solu tion (concentration of  0.01 mol/L) until the 
solution changes from red to green; carry out  a blank determination at the same time. 
4.6.3 Calculations 
Use the following formula (4) to calc ulate the acidity of the sample - ω
3:   
    c × (V 1 – V 0) × M 
  ω3 =  ------------- ----------- ×   100 …………….(4) 
     1000 m 
Where: ω
3  =the mass percentage of the sample’s acid content expressed as a %: 
c   =the concentration of the sodium  hydroxide titrate solution (mol/L) 
V1 = the amount of titrate cons umed during the assay (mL) 
V0 = the amount of titrate consumed during the blank assay (mL)  
m  = mass of the sample (g)           
M  = hydrochloric molar mass (g/moL), [M ___ H 2SO 4]=49.04].               
4.7  Determination of water content  
Using the GB/T1600 Karl Fischer technique faci litates the use of highly precise moisture 
measurement instruments. 
4.8 Testing and required tolerances 
Carry out using the GB/T 1604 parameters. 
5 Labelling, marking, packaging, transit,  storage, safety and certification 
period 
5.1 Labelling, marking and packaging 
The labelling, marking and packaging of d-allethrin should conform to the requirements 
stipulated in general rule GB 3796. It s hould be contained in plastic coated metal 
containers, each weighing between 20-50kg. It can  be packaged in a different manner 
according to user’s requirements but th e packaging must conform to GB 3796. 
5.2 Storage and shipping 
Containers of d-allethrin should be stored  in a suitable dry, ventilated room; during 
shipping, care must be taken to ensure the containers are protected from moisture and 
sunlight. The containers should not be shipped together with foodstuffs, seeds or animal 
feed and should not come into contact with sk in or eyes. Take measures to ensure none 
of the contents are ingested orally or  inhaled. 
5.3 Safety 
D-allethrin is classified  as a low-toxicity insecticide. Pr otective clothing  should be worn 
when using this product and users should wa sh with soap after handling. This product 
has no particular and effective antidote. The main form of treatment is thoroughly rinsing 
off any trace and treating on a case by case basis. 
5.4 Effective inspection period  
The effective inspection period of d-allethrin is one month. Quality inspections which 
test for conformity with relevant standards should be carried out within one month of 
receipt. 
 Annex A 
(Informative annex) 
Alternative names for d-allethrin, structur al formula and basic material statistics 
 
The chemical name, common name, structural formula and basic mate rial statistics of d-
allethrin are as follows: 
ISO common name:  d-allethrin CIPAC reference code: 742 
CASE registry No:  584-79-2 
Chemical name:  (RS)-3-allyl-2-met hyl-4-oxocyclopent-2-enyl (1R)-cis,  
    transchrysanthemate 
Structural formula:   
  
Molecular formula:   C 19H26O3 
Relative molecular mass: 302.41 (according to  2007 internationa l relative atomic 
mass) 
Bioactivity:   Pesticide Vapour pressure (21.6ºC): 1.65 × 10 
-4Pa  
Solubility   Not soluble in water. Miscible with most other organic  
    solvents including acetone, dimethylbenzene, chloroform  
    and ethanol. Stability:    Stable in the presen ce of weak-mild acid ity; easily breaks  
    down in the presence of an  alkali; becomes instable if  
    exposed to sunlight.