PDF GB/T 18414-2025 English (GB/T 18414.1-2006: Older version)
Search result: GB/T 18414-2025 (GB/T 18414.1-2006 Older version)
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Name of Chinese Standard | Status |
| GB/T 18414-2025 | English | 260 |
Add to Cart
|
0-9 seconds. Auto-delivery.
|
Textiles - Determination of chlorinated phenols and ortho-phenylphenol
| Valid |
| GB/T 18414.1-2006 | English | 70 |
Add to Cart
|
0-9 seconds. Auto-delivery.
|
Textiles - Determination of the content of chlorinated phenols - Part 1: Gas chromatography/mass spectrography
| Valid |
| GB/T 18414.1-2001 | English | 279 |
Add to Cart
|
3 days
|
Textiles -- Determination of the residues of pentachlorophenol -- Part 1: Gas chromatography/mass spectrography
| Obsolete |
PDF Preview: GB/T 18414-2025 PDF Preview: GB/T 18414.1-2006
GB/T 18414-2025: PDF in English (GBT 18414-2025) GB/T 18414-2025
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 59.080.01
CCS W 04
Replacing GB/T 18414.1-2006, GB/T 18414.2-2006 and GB/T 20386-2006
Textiles - Determination of Chlorinated Phenols and Ortho-
phenylphenol
ISSUED ON. FEBRUARY 28, 2025
IMPLEMENTED ON. MARCH 1, 2027
Issued by. State Administration for Market Regulation;
Standardization Administration of the People’s Republic of China.
Table of Contents
Foreword... 3
1 Scope... 5
2 Normative References... 5
3 Terms and Definitions... 5
4 Principle... 5
5 Reagents and Materials... 5
6 Instruments and Equipment... 7
7 Specimen Preparation... 7
8 Test Steps... 7
9 Quantitation Limits, Recovery Rates and Precision... 9
10 Test Report... 9
Appendix A (normative) Basic Information of Chlorinated Phenols and Ortho-
phenylphenol... 11
Appendix B (informative) Example of Gas Chromatography-Mass Spectrometry (GC-
MS) Analysis Test Parameters... 12
Appendix C (informative) Total Ion Chromatogram of GC-MS Analysis of Acetylated
Chlorinated Phenols and Ortho-phenylphenol Standard Substances / Standard Samples
... 15
Appendix D (informative) Spiked Recovery Rate of Negative Samples... 17
Textiles - Determination of Chlorinated Phenols and Ortho-
phenylphenol
WARNING. personnel using this document shall have practical experience in formal
laboratory work. This document does not address all possible safety issues. The user is
responsible for taking appropriate safety measures and ensuring compliance with the
conditions stipulated by relevant national laws and regulations.
1 Scope
This document describes the determination method for 19 chlorinated phenols and ortho-
phenylphenol in textiles by gas chromatograph-mass spectrometer (GC-MS).
This document applies to all kinds of textile products.
2 Normative References
The contents of the following documents constitute indispensable clauses of this document
through the normative references in the text. In terms of references with a specified date, only
versions with a specified date are applicable to this document. In terms of references without a
specified date, the latest version (including all the modifications) is applicable to this document.
GB/T 6682 Water for Analytical Laboratory Use - Specification and Test Methods
3 Terms and Definitions
This document does not have terms or definitions that need to be defined.
4 Principle
After the specimen is ultrasonically extracted by potassium hydroxide / methanol solution, it is
derivatized by acetic anhydride and extracted by n-hexane, and then, determined by gas
chromatography-mass spectrometry using the internal standard method.
5 Reagents and Materials
Unless otherwise specified, all reagents used are of analytical grade.
5.1 n-Hexane. CAS No.. 110-54-3, chromatographically pure.
5.2 Water. Grade-3 water specified in GB/T 6682.
5.3 Acetic anhydride. CAS No.. 108-24-7.
5.4 Anhydrous sodium sulfate. CAS No.. 7757-82-6.
5.5 Chlorinated phenols and ortho-phenylphenol standard substances / standard samples. purity
97% (mass fraction), in accordance with the provisions of Appendix A.
5.6 2-Chlorophenol-d4 (internal standard 1). CAS No.. 93951-73-6, purity 97% (mass
fraction).
5.7 2,4-Dichlorophenol-d3 (internal standard 2). CAS No.. 93951-74-7, purity 99% (mass
fraction).
5.8 2,3,4,6-Tetrachlorophenol-13C6 (internal standard 3). CAS No.. 1246820-81-4, purity 98%
(mass fraction).
5.9 Pentachlorophenol-13C6 (internal standard 4). CAS No.. 85380-74-1, purity 98% (mass
fraction).
5.10 Potassium hydroxide solution. weigh-take an appropriate amount of potassium hydroxide
and use water to prepare it into 2 mol/L potassium hydroxide solution.
5.11 Standard stock solution. respectively weigh-take appropriate amounts of chlorinated
phenols and ortho-phenylphenol standard substances / standard samples (5.5) (accurate to 0.1
mg) and use acetonitrile (chromatographically pure) to prepare them into 1,000 mg/L stock
solution.
NOTE. the standard stock solution is stored in an environment of 0 C ~ 4 C and has a validity
period of 6 months.
5.12 Mixed standard working solution. pipette an appropriate amount of the standard stock
solution (5.11) of chlorinated phenols and ortho-phenylphenol and use potassium hydroxide
solution (5.10) to prepare it into 10 mg/L mixed working solution.
NOTE. the mixed standard working solution is stored in an environment of 0 C ~ 4 C and has a
validity period of 1 month.
5.13 Internal standard stock solution. weigh-take an appropriate amount of the internal standard
(5.6 ~ 5.9) (accurate to 0.1 mg) and use potassium hydroxide solution (5.10) to prepare it into
100 mg/L internal standard stock solution.
NOTE. the internal standard stock solution is stored in an environment of 0 C ~ 4 C and has a
validity period of 6 months.
5.14 Extraction solution. respectively pipette an appropriate amount of the internal standard
stock solution (5.13), add an appropriate amount of methanol (chromatographically pure), and
use potassium hydroxide solution (5.10) to prepare it into potassium hydroxide / methanol
(volume ratio 1.1) extraction solution containing 10 g/L internal standard.
5.15 Organic phase needle filter. with a pore size of 0.45 m.
6 Instruments and Equipment
6.1 Gas chromatograph-mass spectrometer (GC-MS). equipped with electron impact ionization
source (EI).
6.2 Analytical balance. respectively with an accuracy of 0.1 mg and 0.01 g.
6.3 Ultrasonic water bath generator. controllable temperature (70 5) C, operating frequency
(40 5) kHz.
6.4 Vortex mixer.
6.5 Mechanical oscillator. the oscillation frequency is about 200 times/min (one reciprocating
motion is 1 time), and the horizontal amplitude is 2 cm ~ 5 cm.
6.6 Pipette. 1 mL ~ 10 mL, 10 L ~ 100 L.
6.7 Extraction bottle. about 50 mL, made of hard glass, with a stopper.
7 Specimen Preparation
Select a sufficient amount of representative sample, cut it into pieces with a maximum size not
exceeding 5 mm, evenly mix them, and use an analytical balance (6.2) to accurately weigh-take
1.0 g (accurate to 0.01 g) from them as the specimen for later use.
8 Test Steps
8.1 Extraction
Place the specimen prepared in 7 in an extraction bottle (6.7), add 20 mL of extraction solution
(5.14), then, seal the stopper, and in an ultrasonic generator (6.3) in a (70 5) C water bath,
extract it for 2 h 5 min.
8.2 Acetylation
After the extraction is completed, take out the above-mentioned extraction bottle, cool it to
room temperature, and add 2 mL of acetic anhydride (5.3). Use a vortex mixer (6.4) to vortex
and oscillate it for 1 min, then, add 2.0 mL of n-hexane (5.1), use a mechanical oscillator (6.5)
to mechanically oscillate it for 30 min at room temperature, and let it stand for stratification.
Add an appropriate amount of anhydrous sodium sulfate (5.4), take part of the supernatant
liquid and filter it through an organic phase needle filter (5.15) into a sampling bottle for GC-
MS determination (8.4).
8.3 Acetylation of Standard Working Solution
Use a pipette (6.6) to pipette a certain volume of the mixed standard working solution (5.12)
into an extraction bottle (6.7), add 20 mL of extraction solution (5.14), and in accordance with
the steps of 8.2, handle it. Prepare at least 5 concentrations of acetylated standard working
solutions (such as. 0.02 mg/L, 0.05 mg/L, 0.2 mg/L, 0.5 mg/L and 1.0 mg/L).
8.4 Gas Chromatography-Mass Spectrometry
8.4.1 Analysis conditions
Appendix B gives an example of gas chromatography-mass spectrometry (GC-MS) analysis
test parameters.
8.4.2 Qualitative analysis
Under the analysis conditions of 8.4.1, by comparing the retention time of the specimen solution
with that of the standard working solution (the retention time deviation tolerance is 0.1 min),
in addition, in the mass spectrum of the sample after background subtraction, the reference
qualitative ions shall all appear, and the abundance ratio of the qualitative ions shall be
consistent with the relative abundance ratio of the standard working solution with an equivalent
concentration (see Appendix B), then, it can be determined that the corresponding analyte is
present in the sample.
The total ion chromatogram of GC-MS analysis of acetylated chlorinated phenols and ortho-
phenylphenol standard substances / standard samples is shown in Appendix C.
8.4.3 Quantitative analysis
In accordance with the content of the analyte in the specimen, select the standard working
solution with similar response value and use the internal standard method for quantitative
analysis. Take the ratio of the peak area of the target compound under the quantitative ion
channel to the peak area of the corresponding internal standard as the vertical axis, and the ratio
of the concentration of the target compound to the concentration of the corresponding internal
standard as the horizontal axis to draw the standard working curve. The response values of the
target substances in the specimen solution shall all be within the linear range of the instrument
detection. If they exceed the range of the standard working curve, the specimen solution shall
be diluted to an appropriate concentration before analysis.
8.5 Blank Test
Except that no specimen is added, carry out the test in accordance with the steps 8.1 ~ 8.4.
8.6 Result Calculation
In accordance with Formula (1), respectively calculate the contents of chlorinated phenols and
ortho-phenylphenol. The calculation result shall retain two decimal places.
Appendix B
(informative)
Example of Gas Chromatography-Mass Spectrometry (GC-MS) Analysis Test
Parameters
Since the test results depend on the instruments used, it is not possible to give general
parameters for chromatographic analysis. The set parameters shall ensure that the component
under test can be effectively separated from other components when determined under
chromatographic conditions. The following parameters are proven to be feasible.
a) Capillary chromatography column. DB-23, 30 m 0.25 mm 0.25 m or equivalent;
b) Inlet temperature. 250 C;
c) Heating program. initial temperature 50 C, maintain for 1 min, at 10 C/min, raise to
180 C, maintain for 1 min, then, at 12 C/min, raise to 240 C, maintain for 2 min;
d) Ion source temperature. 230 C;
e) Mass spectrometer interface temperature. 280 C;
f) Determination mode. selected ion monitoring (SIM); selected ions are shown in Table
B.1;
g) Injection mode. splitless injection;
h) Solvent delay time. 10.5 min;
i) Carrier gas. helium 99.999% (volume fraction), flow rate 1.2 mL/min;
j) Injection volume. 1.0 L;
k) Ionization mode. EI;
l) Ionization energy. 70 eV.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
|