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04/2015:20540 Column :
material : fused silica ;
size : l = 30 m, = 0.25 mm ;
stationary phase : polar-deactivated polyethyleneglycol R
(lm thickness 1 m).
Carrier gas : helium for chromatography R.
METHOD
Head-space gas chromatography (2.2.28) coupled with mass
spectrometry (2.2.43). Prepare the test solution and reference
solutions immediately before use.
Solvent mixture : water R, acetonitrile R (20:80 V/V). The use
of acetonitrile of appropriate purity is essential.
Solution A. Dissolve 30 mg of anhydrous sodium thiosulfate R
and 60.0 g of sodium iodide R in water R using sonication and
dilute to 50.0 mL with the same solvent.
Internal standard solution. Dilute 10 L of butyl
methanesulfonate CRS (BMS) to 10.0 mL with the solvent
mixture. Dilute 20 L of the solution to 100.0 mL with the
solvent mixture.
Blank solution. Introduce 0.5 mL of solution A and 0.5 mL of
the internal standard solution into a headspace vial and seal
the vial immediately with a polytetrauoroethylene-coated
silicon membrane and an aluminium cap.
Test solution. Weigh 25.0 mg of the substance to be examined
into a 20 mL headspace vial. Add 0.50 mL of solution A and
0.50 mL of the internal standard solution and seal the vial
immediately with a polytetrauoroethylene-coated silicon
membrane and an aluminium cap.
Following the derivatisation reaction, a precipitate may be
observed, however this does not affect the validity of the
quantification.
Reference solution (a). Dissolve 25.0 mg each of methyl
toluenesulfonate R (MTS), ethyl toluenesulfonate R (ETS) and
isopropyl toluenesulfonate R (ITS) in toluene R and dilute to
5.0 mL with the same solvent. Dilute 50 L of the solution to
25.0 mL with the internal standard solution.
Reference solution (b). Dilute 40 L of reference solution (a)
to 20.0 mL with the internal standard solution. Introduce
0.50 mL of this solution and 0.50 mL of solution A into a
20 mL headspace vial and seal the vial immediately with
a polytetrauoroethylene-coated silicon membrane and an
aluminium cap.
Reference solution (c). Dilute 500 L of reference solution (a)
to 20.0 mL with the internal standard solution. Introduce
0.50 mL of this solution and 0.50 mL of solution A into a
20 mL headspace vial and seal the vial immediately with
a polytetrauoroethylene-coated silicon membrane and an
aluminium cap.
General Notices (1) apply to all monographs and other texts
Temperature :
Column
Time
(min)
0-1
Temperature
(C)
40
1 - 10
40 130
220
Injection port
Detector
transfer line
280
source
250
analyser
200
Qualication ion
(m/z)
127
142
127
156
127
170
127
Substance
Butyl iodide (BuI)*
* formed from BMS, MTS, ETS and ITS in the derivatisation reaction.
4501
A1
A2
C
4502
I1