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GB/T 33611-2017 (GB/T33611-2017)

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GB/T 33611-2017: PDF in English (GBT 33611-2017)
GB/T 33611-2017
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 59.080.01
W 04
Textiles – Determination of Short Chain
4-(1,1,3,3-Tetramethylbutyl) Phenol Ethoxylate
ISSUED ON. MAY 12, 2017
IMPLEMENTED ON. OCTOBER 1, 2017
Issued by. General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of PRC.
3. No action is required - Full-copy of this standard will be automatically &
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Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative References ... 4
3 Principle ... 4
4 Reagent and Standard Solution ... 5
5 Apparatus and Materials ... 5
6 Sample Pre-Treatment ... 6
7 Determination ... 6
8 Result Calculation ... 7
9 Determination Low Limit of Method and Precision ... 8
10 Test Report ... 8
Appendix A (Informative) Normal Phase HPLC Reference Retention Time and
Chromatogram of Short Chain 4-(1,1,3,3-Tetrametylbutyl) Phenol Ethoxylate
Standard Product ... 9
Foreword
This Standard was drafted as per the rules specified in GB/T 1.1-2009.
This Standard was proposed by China National Textile and Apparel Council.
This Standard shall be under the jurisdiction of National Technical Committee for
Standardization of Textiles (SAC/TC 209).
Drafting organizations of this Standard. Ningbo Inspection and Quarantine Institute of
Science and Technology, CTTC Inspection and Certification Co., Ltd., Ningbo Yinzhou
China Inspection Co., Ltd., and Haosha Industry (Fujian) Co., Ltd.
Chief drafting staffs of this Standard. Bao Qibei, Fu Kejie, Zhang Hui, Ren Qingqing,
Qian Dan, Lian Cefeng, Xu Jianlin, Yang Lisheng, Feng Yun, Fu Chunlin, and Chang
Xiangzhen.
Textiles – Determination of Short Chain
4-(1,1,3,3-Tetramethylbutyl) Phenol Ethoxylate
Warning – Personnel using this Standard shall have practical working
experience in the formal laboratory. This Standard doesn’t indicate all possible
safety issues. The users shall be responsible for taking appropriate safety and
health measures, and ensure to conform to the specified conditions of relevant
national regulations.
1 Scope
This Standard specifies the method of adopting the normal phase High Performance
Liquid Chromatography (HPLC) to determine the 3 kinds of short chain 4-(1, 1, 3, 3-
tetrametylbutyl) phenol ethoxylate, namely, 4-tert-octylphenol monoethoxylate, 4-tert-
octylphenol diethoxylate, 4-tert-octylphenol triethoxylate in the textiles.
This Standard is applicable to all types of textile products.
2 Normative References
The following documents are essential to the application of this document. For the
dated documents, only the versions with the dates indicated are applicable to this
document; for the undated documents, only the latest version (including all the
amendments) are applicable to this document.
GB/T 6682 Water for Analytical Laboratory Use – Specification and Test Methods
3 Principle
Take methanol as the extraction solvent; use ultrasonic wave to extract short chain 4-
(1, 1, 3, 3-tetrametylbutyl) phenol ethoxylate in the specimen; concentrate the
extracting solution, then use normal phase high performance liquid chromatography
with fluorescence detector to determine; use external standard method to determine
the quantity.
6 Sample Pre-Treatment
Select the representative sample; cut into 5mm × 5mm pieces, mix evenly. Weigh 2g
of specimen, accurate to 0.01g; place into the stoppered conical flask (5.4); add 50mL
of methanol (4.1), extract for 40min under the room temperature in the ultrasonic-wave
generator (5.2); transfer the extracting solution into the round bottom flask (5.5); then
use 10mL of methanol (4.1) to wash the slag, add into the extracting solution.
Concentrate to 1mL at 40°C rotary evaporator (5.6); then use isopropanol (4.3) to make
the constant volume of 10mL. Filter the solution through the organic phase filter
membrane (5.7), then serve as the sample solution to be tested by the normal phase
high performance liquid chromatography.
7 Determination
7.1 Normal phase high performance liquid chromatography conditions
Since the test results depend on the instrument used; it is not possible to give general
parameters for chromatographic analysis. The following parameters have been proved
to be appropriate for the test.
a) Chromatographic column. Dikma platisil silica gel column; 250mm × 4.6mm,
5.0µm or equivalent.
b) Chromatographic column temperature. 35°C.
c) Mobile phase.
--- Mobile Phase A. n-hexane + isopropanol (85.15);
--- Mobile Phase B. isopropanol + water (85.15).
d) Fluorescence detector. excitation wavelength of 230nm; emission wavelength of
296nm.
e) Flow rate. 0.5mL/min.
f) Sample injection volume. 10µL.
g) Gradient elution program, refer to Table 1.
......
 
(Above excerpt was released on 2017-09-15, modified on 2021-06-07, translated/reviewed by: Wayne Zheng et al.)
Source: https://www.chinesestandard.net/PDF.aspx/GBT33611-2017