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GB/T 36922-2018 English PDF (GBT36922-2018)

GB/T 36922-2018 English PDF (GBT36922-2018)

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GB/T 36922-2018: Determination of organophosphorous flame retardants in toys -- Gas chromatography-mass spectrography method

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.
GB/T 36922-2018
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 97.200.50
Y 57
Determination of organophosphorus flame retardants
in toys - Gas chromatometry-mass spectrometry
method
ISSUED ON: DECEMBER 28, 2018
IMPLEMENTED ON: DECEMBER 28, 2018
Issued by: State Administration for Market Regulation;
Standardization Administration of the People's Republic of
China.
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
method
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??0.25??m, or
equivalent;
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: 1??L;
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):
Where,
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
precision
7.1 Lower limit of quantitation
The three organic phosphorus flame retardant methods have a lower limit of 1mg/kg.
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 85%~110%.

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