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GB/T 36922-2018 PDF in English

GB/T 36922-2018 (GB/T36922-2018, GBT 36922-2018, GBT36922-2018)
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GB/T 36922-2018: PDF in English (GBT 36922-2018)

GB/T 36922-2018
ICS 97.200.50
Y 57
Determination of organophosphorus flame retardants
in toys - Gas chromatometry-mass spectrometry
Issued by: State Administration for Market Regulation;
Standardization Administration of the People's Republic of
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Principle ... 4 
3 Reagents and materials ... 4 
4 Instruments and devices ... 5 
5 Analysis steps ... 5 
6 Result calculation ... 8 
7 Lower limit of quantitation, recovery rate and precision ... 8 
8 Test report ... 9 
Annex A (informative) Chromatogram of organic phosphorus flame retardant
... 10 
Annex B (informative) Precision ... 11 
Bibliography ... 12 
Determination of organophosphorus flame retardants
in toys - Gas chromatometry-mass spectrometry
WARNING - Personnel using this Standard shall have practical experience
in formal laboratory work. This Standard does not indicate all possible
safety issues. It is the user's responsibility to take appropriate safety and
health measures and to ensure compliance with the conditions
prescribed by the relevant national regulations.
1 Scope
This Standard specifies gas chromatometry-mass spectrometry method for
three organic phosphorus flame retardants: tris(2-chloroethyl) phosphate
(TCEP), tris(1,3-dichloroisopropyl) phosphate (TDCP) and tris(2-chloro-1-
methylethyl) phosphate (TCPP) in toys.
This Standard is applicable to determination of organic phosphorus flame
retardant in polymer materials in toys.
2 Principle
Use toluene to extract TCEP, TDCP and TCPP in the sample in Soxhlet
extractor. After setting the volume of the extract, use gas chromatography-mass
spectrometry (GC-MS) to determine. Use external standard method to quantify.
3 Reagents and materials
3.1 Toluene.
3.2 TCEP standard product: purity is not less than 97%.
3.3 TDCP standard product: purity is not less than 97%.
3.4 TCPP standard: purity not less than 95%.
3.5 Standard stock solution: Accurately weigh TCEP standard products (see
3.2), TDCP standard products (see 3.3) and TCPP standard products (see 3.4).
Use toluene (see 3.1) to prepare 1000mg/L stock solution.
Take test solution. Filter through the membrane filter (see 4.3). Conduct gas
chromatography-mass spectrometry analysis.
Soxhlet extraction process: The temperature shall be controlled at the reflux
temperature of toluene, about 110°C. Rotary evaporator water bath
temperature is 40°C ~ 50°C. At the same time, keep the pressure between 5
kPa~8 kPa.
5.4 Gas chromatometry-mass spectrometry method
5.4.1 GC-MS determination conditions
Different GC-MS has different analysis parameters. The set parameters shall
ensure that the measured component can be effectively separated from other
components during the measurement. The following parameters are one of the
GC-MS measurement conditions:
a) Chromatography column: HP-5MS column, 30m×0.25mm×0.25μm, or
b) Inlet temperature: 300°C;
c) Chromatography-mass spectrometer interface temperature: 280°C;
d) Sampling method: pressure-splitless injection. Apply a pressure of
344.75kPa. Open the valve after 1.0min;
e) Carrier gas: helium, purity ≥99.999%; control mode: constant flow; flow
rate: 1.8mL/min;
f) Temperature programming: After maintaining at 80°C for 2min, raise to
160°C at 20°C/min. Maintain 1min. Then raise to 320°C at 40°C/min.
Maintain 2min;
g) Injection volume: 1μL;
h) Ion source: EI source;
i) Ionization energy: 70eV;
j) Scanning method: Select ion monitoring (SIM);
k) Quadrupole temperature: 150°C;
l) Ion source temperature: 230°C;
m) Solvent delay time: 3min.
The chromatogram of each standard under the above measurement conditions
6 Result calculation
If it is determined that TCEP, TDPP, and TCPP are present, perform external
standard quantitative analysis based on the extracted ion chromatographic
peak area. The content of TCEP, TDPP and TCPP in the sample is calculated
according to formula (1):
Xi - The content of organic phosphorus flame retardant in the sample, in
milligrams per kilogram (mg/kg);
CS - The concentration of organic phosphorus flame retardant in the test
solution, in milligrams per liter (mg/L);
V - The set volume of toluene, in milliliters (mL);
D - The dilution factor;
m - The mass of test material, in grams (g).
Calculate the concentration of organic phosphorus flame retardant in the
sample according to the above formula. If the test response value of the test
solution exceeds the linear range, it shall be appropriately diluted and
measured. The result is kept to one decimal place.
7 Lower limit of quantitation, recovery rate and
7.1 Lower limit of quantitation
The three organic phosphorus flame retardant methods have a lower limit of
7.2 Recovery rate
Quantitatively add an appropriate standard solution of known concentration to
the sample. Perform recovery rate analysis according to the above test steps
5.2~5.4. The recovery rate of TCEP, TDPP and TCPP in the polymer shall be
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.