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GB/T 18414.1-2006 English PDF (GBT18414.1-2006)

GB/T 18414.1-2006 English PDF (GBT18414.1-2006)

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GB/T 18414.1-2006: Textiles -- Determination of the content of chlorinated phenols -- Part 1: Gas chromatography/mass spectrography

This Part of GB/T 18414 specifies the use of gas chromatography-mass selective detector (GC-MSD), for the determination of chlorophenols (2,3,5,6-tetrachlorophenol and pentachlorophenol), as well as their salts and phenols, in textiles. This Part applies to textile materials and their products.
GB/T 18414.1-2006
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 59.080.01
W 04
Replacing GB/T 18414.1-2001
Textiles - Determination of the content of chlorinated
phenols - Part 1: Gas chromatography/mass
spectrography
ISSUED ON: MAY 25, 2006
IMPLEMENTED ON: DECEMBER 01, 2006
Issued by: General Administration of Quality Supervision, Inspection and Quarantine of PRC;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Principles ... 4
4 Reagents and materials ... 5
5 Instrument and equipment ... 5
6 Analytical procedures ... 6
7 Result calculation ... 7
8 Low limit of determination, recovery rate, precision ... 8
9 Test report ... 8
Appendix A (Normative) Types of chlorinated phenol ... 10
Appendix B (Informative) Quantitative and qualitative selective ion for chlorophenol acetate ... 11
Appendix C (Informative) ... 12
Gas chromatography-mass spectrometry selective ion chromatogram (GC-
MSD) of chlorinated phenol acetate standard ... 12
Appendix D (Informative) Gas chromatography-mass spectrogram ... 13
Textiles - Determination of the content of chlorinated
phenols - Part 1: Gas chromatography/mass
spectrography
Warning - The personnel using this part of GB/T 18414 shall have practical experience in formal laboratory work. This standard does not point out all possible safety issues. The user is responsible for taking appropriate
safety and health measures AND ensuring compliance with the conditions
stipulated by relevant national laws and regulations.
1 Scope
This Part of GB/T 18414 specifies the use of gas chromatography-mass
selective detector (GC-MSD), for the determination of chlorophenols (2,3,5,6- tetrachlorophenol and pentachlorophenol), as well as their salts and phenols, in textiles.
This Part applies to textile materials and their products.
2 Normative references
The provisions in following documents become the provisions of this Part through reference in this Part of GB/T 18414. For the dated references, the subsequent amendments (excluding corrections) or revisions do not apply to this Part; however, parties who reach an agreement based on this Part are encouraged to study if the latest versions of these documents are applicable. For undated references, the latest edition of the referenced document applies. GB/T 6682 Water for analytical laboratory use - Specification and test
methods (GB/T 6682-1992, neq ISO 3696:1987)
3 Principles
The specimen is extracted by potassium carbonate solution. The extract is acetylated by acetic anhydride; extracted by n-hexane; measured by a gas chromatograph (GC-MSD), which is equipped with a mass selective detector; confirmed by selective ion detection; quantified by external standard method. 4 Reagents and materials
Unless otherwise specified, the reagents used are all analytically pure; the water is grade-2 water, that meets the requirements of GB/T 6682.
4.1 n-hexane.
4.2 Acetic anhydride.
4.3 Anhydrous potassium carbonate.
4.4 Anhydrous sodium sulfate: Burn at 650 ??C for 4 h; store it in a desiccator for later use, after cooling.
4.5 Potassium carbonate solution: 0.1 mol/L aqueous solution; dissolve 13.8 g of anhydrous potassium carbonate in water; make the volume reach to 1000 mL.
4.6 Sodium sulfate solution: 20 g/L.
4.7 The 2,3,5,6-tetrachlorophenol standard and the pentachlorophenol
standard: Purity ??? 99%, as shown in Appendix A.
4.8 Standard stock solution: Weigh appropriate amounts of 2,3,5,6-
tetrachlorophenol standard and pentachlorophenol standard, respectively. Use potassium carbonate solution to prepare a standard stock solution, which has a concentration of 100 ??g/mL.
4.9 Mixed standard working solution: Use potassium carbonate solution, to dilute it to a mixed standard working solution, which has suitable concentration, as required.
Note: The shelf life of the standard stock solution, in the refrigerator at 0 ??C ~ 4 ??C, is 6 months. The shelf life of the mixed standard working solution, in the refrigerator at 0 ??C ~ 4 ??C, is 3 months.
5 Instrument and equipment
5.1 Gas chromatograph: It is equipped with a mass selective detector (MSD). 5.2 Ultrasonic generator: The working frequency is 40 kHz.
5.3 Centrifuge: 4000 r/min.
5.4 Separation funnel: 150 mL.
c) Sample inlet temperature: 270 ??C;
d) Chromatography mass spectrometer's interface temperature: 260 ??C;
e) Carrier gas: nitrogen, purity ??? 99.999%, 1.4 mL/min;
f) Ionization method: El;
g) Ionization energy: 70 eV;
h) Measurement method: Selective ion monitoring method, see Appendix B; i) Sample injection mode: Splitless injection; open the valve after 1.2 min; j) Sample injection volume: 1 ??L.
6.4.2 Gas chromatography-mass spectrometry determination and
confirmation of positive results
According to the content of the analyte in the sample solution, select a standard working solution (6.3), which has a similar concentration. According to the conditions of 6.4.1, measure the standard working solution and the sample solution, by injecting sample of equal volumes. The response values of 2,3,5,6- tetrachlorophenol acetate and pentachlorophenol acetate, in the standard working solution and the sample solution, shall be within the linear range of the instrument detection.
Note: Under the above-mentioned gas chromatography-mass spectrometry conditions, the gas chromatography-mass spectrogram's selective ion chromatograms of 2,3,5,6- tetrachlorophenol acetate and pentachlorophenol acetate, are as shown in Figure C. 1 in Appendix C. For gas chromatography-mass spectrogram, please refer to Figure D.1 in Appendix D.
If there are chromatographic peaks in the selected ion chromatograms of the sample solution and the standard working solution, at the same retention time, THEN, it is confirmed according to the types of selective ions and their abundance ratios in Appendix B.
7 Result calculation
The content of chlorophenol, in the specimen, is calculated by formula (1). The result is expressed to two decimal places:
Where:
Xi - The content of chlorophenol i in the specimen, in milligrams per kilogram (mg/kg);
Ai - The peak area (or peak height) of chlorophenol acetate i, in the sample solution;
Ais - The peak area (or peak height) of chlorophenol acetate i, in the standard working solution;
ci - The concentration of chlorophenol i in the standard working solution, in milligrams per liter (mg/L);
V - The volume of the sample solution, in milliliters (mL);
m - The specimen volume, which is represented by the final sample solution, in grams (g).
8 Low limit of determination, recovery rate, precision
8.1 Lower limit of determination
The lower limit of determination of this method is 0.05 mg/kg, for 2,3,5,6- tetrachlorophenol and pentachlorophenol.
8.2 Recovery rate
When 2,3,5,6-tetrachlorophenol and pentachlorophenol are in the range of 0.05 mg/kg ~ 2.00 mg/kg, the recovery rate is 85% ~ 110%.
8.3 Precision
In the same laboratory, the absolute difference between the two independent test results, which are obtained by the same operator, using the same
equipment AND the same test method, performing independent tests on the same object under test, within a short period of time, is not greater than 10% of the arithmetic mean of the two measurement values, based on the condition that those more than 10% of the arithmetic mean of the two measured values does not exceed 5%.
9 Test report
The test report shall at least provide the following:
a) Specimen description;
b) Standards used;

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