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GB/T 42696-2023: Textiles -- Determination of phosphate compounds
GB/T 42696-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 59.080.01
CCS W 04
Textiles - Determination of phosphate compounds
ISSUED ON: MAY 23, 2023
IMPLEMENTED ON: DECEMBER 1, 2023
Issued by: State Administration for Market Regulation;
Standardization Administration of the PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Terms and definitions ... 4
4 Principle ... 4
5 Reagents and materials ... 4
6 Apparatus ... 5
7 Analytical procedure ... 6
8 Calculation and presentation of results ... 9
9 Limit of quantification and precision ... 9
10 Test report ... 10
Appendix A (Informative) Gas chromatogram of phosphate compound standard
substances ... 11
Appendix B (Informative) Gas chromatography-mass spectrometry selected ion
chromatogram of phosphate compound standard substances ... 12
Textiles - Determination of phosphate compounds
Warning - Personnel using this document shall have practical experience in
regular laboratory work. This document does not purport to address all possible
safety problems. Users are responsible for taking appropriate safety and health
measures AND ensuring the conditions specified in relevant national regulations.
1 Scope
This document describes the gas chromatography and gas chromatography-mass
spectrometry methods for the determination of the content of 8 phosphate compounds
in textiles.
This document applies to all types of textiles.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
There are no terms or definitions to be defined in this document.
4 Principle
Use ethyl acetate to ultrasonically extract the specimen. After the extract is filtered
through a filter membrane, use a gas chromatograph equipped with a flame photometric
detector (P type) to measure; or use a gas chromatograph-mass spectrometer to measure.
Use the external standard method for quantification.
5 Reagents and materials
Unless otherwise specified, all reagents used are chromatographically pure.
5.1 Tributyl phosphate (TBP): CAS number 126-73-8 (purity≥98.5%).
5.2 Triphenyl phosphate (TPP): CAS number 115-86-6 (purity≥99.7%).
5.3 Tri-o-cresyl phosphate (ToCP): CAS number 78-30-8 (purity≥96%).
5.4 Tri-m-cresyl phosphate (TmCP): CAS number 563-04-2 (purity≥95%).
5.5 Tri-p-cresyl phosphate (TpCP): CAS number 78-32-0 (purity≥98%).
5.6 Trioctyl phosphate (TOP): CAS number 78-42-2 (purity≥98%).
5.7 Diphenyl octyl phosphate (DPOP): CAS number 1241-94-7 (purity≥90%).
5.8 Cresyl diphenyl phosphate (CDP): CAS number 26444-49-5 (purity≥93%).
5.9 Ethyl acetate.
5.10 Standard stock solution: Use ethyl acetate (5.9) to prepare the standard substances
listed in 5.1~5.8 into a single-component standard stock solution with a mass
concentration of approximately 1000 mg/L, respectively.
Note: The standard stock solution is stored in the dark at 0 °C~4 °C and is valid for 6 months.
5.11 Standard working solution: Pipette 8 appropriate amounts of phosphate compound
standard stock solutions (5.10) respectively; place them in the same volumetric flask.
Use ethyl acetate (5.9) to prepare a mixed standard working solution with a mass
concentration of approximately 100 mg/L. Then according to work needs, use ethyl
acetate (5.9) to prepare a standard working solution of appropriate concentration.
Note: The standard working solution is stored in the dark at 0 °C~4 °C and is valid for 3 months.
6 Apparatus
6.1 Gas chromatograph (GC-FPD): It is equipped with flame photometric detector (P
type).
6.2 Gas chromatograph-mass spectrometer (GC-MS): It is equipped with electron
impact ionization source (EI).
6.3 Ultrasonic generator: Working frequency is (40±5)kHz.
6.4 Analytical balance: Graduation values are 0.1 mg and 0.01 g, respectively.
6.5 Vortex mixer.
6.6 Extraction tube: It has an airtight stopper; is about 50 mL; made of hard glass.
6.7 Disposable syringe.
6.8 Organic-phase needle filter head: Pore size is 0.45 μm.
retention times of the specimen solution and the standard working solution, perform
qualitative analysis. Use the chromatographic peak area of the standard substance as
the ordinate; use the concentration of the standard working solution as the abscissa;
draw a standard working curve. Use the external standard method to perform
quantitative analysis.
Note: When the above analysis conditions are used, the GC-FPD (P type) analysis chromatogram
of 8 phosphate compound standard substances are shown in Appendix A. Cresyl diphenyl
phosphate (CDP Ⅰ) and cresyl diphenyl phosphate (CDP Ⅱ) are isomers of each other; the
CDP result is the sum of the isomers.
7.4 Gas chromatography-mass spectrometry analysis method
7.4.1 Gas chromatography-mass spectrometry analysis conditions
Since the test results are related to the instrument and conditions used, it is impossible
to give universal parameters for instrument analysis. The following parameters have
been proven to be suitable for the test.
a) Chromatographic column: HP-5MS, 30 m×0.25 mm×0.25 μm; or equivalent.
b) Column temperature programming:
c) Inlet temperature: 250 °C.
d) Mass spectrometer interface temperature is 250 °C.
e) Ion source temperature: 230 °C.
f) Quadrupole temperature is 150 °C.
g) Ionization method: EI.
h) Ionization energy: 70 eV.
i) Detection method: Selected ion monitoring (SIM) mode; the monitoring ions are
shown in Table 1.
j) Solvent delay: 8 min.
k) Carrier gas: Helium; purity≥99.999%; 1 mL/min.
l) Injection method: Splitless injection; open the valve after 2 min.
m) Injection volume: 1 μL.
8 Calculation and presentation of results
According to formula (1), calculate the content of each phosphate compound in the
specimen. The test results are expressed as the content of each phosphate compound,
respectively. Calculation results are expressed to one decimal place.
Where:
Xi - The content of phosphate compound i in the specimen, in milligrams per kilogram
(mg/kg);
Ci - The mass concentration of the phosphate compound i to be measured in the sample
solution obtained from the standard working curve, in milligrams per liter (mg/L);
Ci0 - The mass concentration of phosphate compound i in the blank specimen solution
in the sample solution obtained from the standard working curve, in milligrams per liter
(mg/L);
V - The final constant volume of sample solution, in milliliters (mL);
m - Specimen mass, in grams (g);
f - Dilution factor.
9 Limit of quantification and precision
9.1 Limit of quantification
The limits of quantification of the 8 phosphate compounds in textiles using the gas
chromatography method are all 2.0 mg/kg. The limits of quantification of the 8
phosphate compounds in textiles using gas chromatography-mass spectrometry are all
1.0 mg/kg.
9.2 Precision
In the same laboratory, by the same operator, using the same equipment, according to
the same test method, the absolute difference between the results of two tests obtained
independently of each other on the same subject within a short period of time IS not
greater than 15% of the arithmetic mean of the two measured values; provided that in
the case of greater than 15%, it does not exceed 5%.