Edifenphos 409: Chemical Name O-Ethyl S, S-Diphenyl Phosphorodithioate (IUPAC

EDIFENPHOS 409
EDIFENPHOS
409
S S
P
O O C2H5
ISO common name Edifenphos

Chemical name O-Ethyl S,S- diphenyl phosphorodithioate (IUPAC,
CA; 17109-49-8)
Empirical formula C14H15O2PS2
RMM 310.4
m.p. 16-17 °C
b.p. 154 °C at 1.3 Pa
v.p. 3.2 × 10-5 Pa at 20 °C
Solubility In water: 47 mg/l at 20 °C; in n-hexane: more than
70 g/l; 2-propanol: more than 600 g/ml; xylene:
600 g/l; octanol: more than 200 g/l, all at 20 °C
Description Technical material is a light to dark yellow liquid
Formulations Emulsifiable concentrates, dustable powders
EDIFENPHOS TECHNICAL
*
409/TC/M/-
1 Sampling. Take at least 100 g.
2 Identity tests
2.1 Infrared. Prepare a sample as a thin film between two KBr windows and adjust
the thickness of the thin film, so that when the IR spectrum is recorded between
4000 cm-1 and 600 cm-1, the transmittance of the major peak at 1239 cm-1 is
between 5% and 10%. The spectrum produced from the sample film should not
differ significantly from that of the standard.
*
CIPAC method 1991. Prepared by the Japanese committee (JAPAC). Chairman: T Suzuki. Based on a method
supplied by Nihon Tokushu Noyaku Seizo K.K., Japan.
79
EDIFENPHOS 409
Characteristic peaks are:
1239 cm-1 P=O

1013 cm-1
1000 cm-1
939 cm-1
} P-O-C
744 cm-1 =C-H monosubstituted aromatic
2.2 GLC. Carry out a gas-liquid chromatographic identity test simultaneously

with the determination of edifenphos. The major peak of the sample should have
the same retention time as that of the standard material.
2.3 TLC. Carry out a thin layer chromatographic identity test by comparing the
sample with the standard using the following conditions:
TLC plate Coated with Silica Gel 60 F254 0.25 mm

(Merck, Darmstadt, FRG)
Solvent Toluene-methylethyl ketone (6:1)
Sample solution An amount of sample containing the equivalent of
10 mg edifenphos is dissolved in approximately 0.5 ml
acetone and made up to 1.0 ml.
Reference solution 10 mg edifenphos standard material is dissolved in
approximately 0.5 ml acetone and made up to 1.0 ml.
Sample size I 10 µl sample solution
Sample size II 5 µl sample solution and 5 µl reference solution.
Allow first the spot to dry before applying the second
solution.
Sample size III 10 µl reference solution
Travelling distance 15 cm
Visualization UV at 254 nm
Rf value Approximately 0.6
The major spot of the sample should have the same R f value as that of the
standard material and the spots in sample II should show single spots.
3 Edifenphos
OUTLINE OF METHOD A solution of the sample is separated by gas-liquid
chromatography. The content of active ingredient is calculated from the peak
area using triphenyl phosphate (TPP) as the internal standard.
80
EDIFENPHOS 409
REAGENTS
Edifenphos standard of known purity
Triphenyl phosphate (TPP) without impurities that disturb the analysis
Acetone RE 34, p. 286
Internal standard solution. Weigh (to the nearest 1 mg) 1.5 g of TPP into a
200 ml volumetric flask, dissolve with sufficient acetone, and dilute to the
volume with acetone.
Calibration solution. Weigh (to the nearest 1 mg) approximately 100 mg
edifenphos standard (s mg) into a 50 ml volumetric flask. Add 10 ml of the
internal standard solution and shake to dissolve. Dilute to the volume with
acetone.
APPARATUS
Gas-liquid chromatograph equipped with a flame ionization detector and an
integrator
Column glass 110 × 3.2 (i.d.) mm packed with 5% Silicone GE SE-30/
Chromosorb W-HP, 80 to 100 mesh
PROCEDURE
(a) Operating conditions (typical):
Column temperature 190 °C
Detector temperature 220 °C
Injection port temperature 220 °C
Carrier gas flow rate, nitrogen 60 ml/min
Retention times About 8.6 and 11.0 min for edifenphos
and internal standard respectively.
(b) Determination. Weigh (to the nearest 1 mg) sufficient sample to contain
approximately 100 mg (w mg) edifenphos into a 50 ml volumetric flask. Add
10 ml of the internal standard solution and shake to dissolve. Dilute to the
volume with acetone (sample solution).
Inject 4 µl portions of the calibration solution until the peak area ratios of
edifenphos to TPP for two successive injections vary less than 1%. Inject a 4 µl
portion of the calibration solution, make duplicate injections of 4 µl portions of
the sample solution, and then inject another 4 µl portion of the calibration
solution. Obtain the peak area ratios of edifenphos to TPP. Average the peak
area ratios of the sample solution injections (R) and also of the calibration
solutions (R') preceding and following the sample injections.
81
EDIFENPHOS 409
(c) Calculation
R s P
Edifenphos content
R' w
where:
s = mass of edifenphos standard in the calibration solution (mg)
w = mass of sample taken (mg)
R' = average peak area ratio of edifenphos to TPP for the calibration
solution
R = peak area ratio of edifenphos to TPP for the sample solution
P = purity of edifenphos standard (g/kg)
Repeatability r = 7.04 g/kg at 950 g/kg active ingredient content

Reproducibility R = 9.10 g/kg at 950 g/kg active ingredient content
EDIFENPHOS EMULSIFIABLE CONCENTRATES

*
409/EC/M/-

2 Identity tests
2.1 GLC. As for 409/TC/M/2.2.
2.2 TLC. AS for 409/TC/M/2.3.
3 Edifenphos. As for edifenphos technical 409/TC/M/3.

EDIFENPHOS DUSTABLE POWDERS

*
409/DP/M/-

2 Identity tests
2.1 GLC. Carry out a gas-liquid chromatographic identity test simultaneously
with the determination of edifenphos. The major peak of the sample should have
the same retention time as that of the standard material.
*
CIPAC method 1991. Prepared by the Japanese committee (JAPAC). Chairman: T Suzuki. Based on a method
supplied by Nihon Tokushu Noyaku Seizo K.K., Japan.
82
EDIFENPHOS 409
2.2 TLC. As for 409/TC/M/2.3, except:

Sample solution. Weigh a sample equivalent to 100 mg of edifenphos into a 50 ml
Erlenmeyer flask with a stopper, add 10 ml acetone and agitate the flask
mechanically for 5 minutes. Filter the solution and collect the filtrate. Take
1.0 ml of the filtrate.
3 Edifenphos. As for edifenphos technical 409/TC/M/3, except:

(b) Determination. Weigh (to the nearest 1 mg) sufficient sample to contain
approximately 100 mg edifenphos (w mg) into a 200 ml Erlenmeyer flask. Add
10 ml of the internal standard solution, 40 ml of acetone, and agitate the flask
mechanically for 20 min. Allow the insoluble material to settle or centrifuge a
portion of the extract to obtain a clear solution. Continue according to
409/TC/M/3 (b) starting at: "Inject 4 µl portions ...."etc.

83

Edifenphos 409: Chemical Name O-Ethyl S, S-Diphenyl Phosphorodithioate (IUPAC

Uploaded by

Copyright:

Available Formats

Edifenphos 409: Chemical Name O-Ethyl S, S-Diphenyl Phosphorodithioate (IUPAC

Uploaded by

Document Information

Original Description:

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Edifenphos 409: Chemical Name O-Ethyl S, S-Diphenyl Phosphorodithioate (IUPAC

Uploaded by

Copyright:

Available Formats

EDIFENPHOS 409

ISO common name Edifenphos

1 Sampling. Take at least 100 g.

Characteristic peaks are:

1239 cm-1 P=O

744 cm-1 =C-H monosubstituted aromatic

2.2 GLC. Carry out a gas-liquid chromatographic identity test simultaneously

TLC plate Coated with Silica Gel 60 F254 0.25 mm

Repeatability r = 7.04 g/kg at 950 g/kg active ingredient content

EDIFENPHOS EMULSIFIABLE CONCENTRATES

1 Sampling. Take at least 500 g.

3 Edifenphos. As for edifenphos technical 409/TC/M/3.

Repeatability r = 9.95 g/kg at 500 g/kg active ingredient content

EDIFENPHOS DUSTABLE POWDERS

1 Sampling. Take at least 500 g.

2.2 TLC. As for 409/TC/M/2.3, except:

3 Edifenphos. As for edifenphos technical 409/TC/M/3, except:

Repeatability r = 0.27 g/kg at 25 g/kg active ingredient content

You might also like

Pfad - The Proxy pFad of © 2024 Garber Painting. All rights reserved.