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Basic data
| Standard ID | SN/T 5244-2020 (SN/T5244-2020) |
| Description (Translated English) | (Import and export textile processing detergents. Determination of alkyl phenol and alkyl phenol polyoxyethylene ether. High performance liquid chromatography) |
| Sector / Industry | Commodity Inspection Standard (Recommended) |
| Classification of Chinese Standard | W04 |
| Classification of International Standard | 59.080.01 |
| Word Count Estimation | 11,177 |
| Date of Issue | 2020-08-27 |
| Date of Implementation | 2021-03-01 |
| Regulation (derived from) | General Administration of Customs Announcement No. 98 [2020] |
| Issuing agency(ies) | General Administration of Customs |
SN/T 5244-2020: (Import and export textile processing detergents. Determination of alkyl phenol and alkyl phenol polyoxyethylene ether. High performance liquid chromatography)
---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Import and export textile processing detergents-Determination of
alkylphenols and alkylphenol polyethoxylates-High performance liquid
chromatography method
The People's Republic of China Entry-Exit Inspection and Quarantine Industry Standards
2020-08-27 release
2021-03-01 implementation
Issued by the General Administration of Customs of the People's Republic of China
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard was proposed and managed by the General Administration of Customs of the People's Republic of China.
Drafting organizations of this standard. Shijiazhuang Customs of the People's Republic of China, Nanjing Customs of the People's Republic of China.
The main drafters of this standard. Zhao Sumin, Gao Youjun, Liu Jinrui, Dou Caiyun, Qian Kai, Jia Haitao, Zhou Jia, Wang Baogang, Cao Shuo
Lei.
Import and export textile processing detergent alkyl phenol and alkyl
Determination of polyoxyethylene phenol ether. High performance liquid chromatography
1 Scope
This standard specifies the high performance liquid chromatography method for the determination of alkylphenols and alkylphenol polyoxyethylene ethers in textile processing detergents.
This standard applies to the determination of alkylphenol and alkylphenol polyoxyethylene ether content in textile processing detergents and products with similar functions.
set.
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article
Pieces. For undated reference documents, the latest version (including all amendments) is applicable to this document.
GB/T 6682 Analytical laboratory water specifications and test methods
GB/T 8170 Numerical rounding rules and the expression and determination of limit values
3 Terms and definitions
The following terms and definitions apply to this document.
3.1
Alkylphenols
The molecular structure of alkylphenol is. R-C6H4-OH. Octylphenol (C8H17-C6H4-OH, OP for short) is common among such substances
And nonylphenol (C9H19-C6H4-OH, referred to as NP).
3.2
Alkylphenol polyethoxylates, APnEO
The molecular structure of alkylphenol polyoxyethylene ether is. R-C6H4-(OC2H4)nOH. Octylphenol polyoxyethylene
Alkenyl ether [C8H17-C6H4-(OC2H4)nOH, referred to as OPnEO] and nonylphenol polyoxyethylene ether [C9H19-C6H4-(OC2H4)nOH, referred to as
NPnEO].
Alkylphenol polyoxyethylene ethers can be used as surfactants in textile processing detergents. Alkylphenols are alkylphenol polyoxyethylene ethers.
4 Principle
The detergent samples were extracted by ultrasonic extraction with methanol as the extraction solvent. After centrifugation, the extraction liquid was
The spectrometer is used for analysis and the external standard method is used for quantification.
5 Reagents and materials
Unless otherwise specified, only use analytically pure reagents and tertiary water or equivalent purity water that meets the requirements of GB/T 6682.
5.1 Methanol. chromatographically pure.
5.2 Acetonitrile. chromatographically pure.
5.3 Octylphenol standard product. OP, purity ≥ 97%.
5.4 Nonylphenol standard product. NP, purity ≥ 99%.
5.5 Standard product of octylphenol polyoxyethylene ether. OPnEO, average degree of polymerization n=9~10, excellent grade pure.
5.6 Nonylphenol polyoxyethylene ether standard product. NPnEO, average degree of polymerization n=9~10, purity ≥ 95%.
5.7 Alkylphenol standard stock solution. accurately weigh appropriate amounts of octylphenol (5.3) and nonylphenol (5.4) standards, and use
Alcohol (5.1) was prepared into a standard stock solution with a concentration of 1 mg/mL.
5.8 Alkylphenol polyoxyethylene ether standard stock solution. accurately weigh appropriate amounts of octylphenol polyoxyethylene ether (5.5) and nonylbenzene respectively
Phenol polyoxyethylene ether (5.6) standard products were prepared with methanol (5.1) to prepare standard stock solutions with a concentration of 1 mg/mL.
5.9 Standard working solution. Pipette the alkylphenol standard stock solution (5.7) and alkylphenol polyoxyethylene with a concentration of 1 mg/mL respectively
Enether standard stock solution (5.8) has an appropriate volume and diluted with methanol (5.1) to prepare a standard working solution of the required concentration.
Note. The standard solution should be stored below 4 ℃ and protected from light. The standard stock solution is valid for 12 months, and the standard working solution is valid for 3 months.
6 Apparatus and equipment
6.1 High performance liquid chromatograph. equipped with fluorescence detector.
6.2 Analytical balance. Sensitivity is 0.1 mg and 0.01 g respectively.
6.3 50 mL plastic centrifuge tube (with lid can be sealed).
6.4 Measuring cylinder. 10 mL.
6.5 Volumetric flask. 25 mL.
6.6 Ultrasonic extraction device. controllable temperature (60 ± 1) ℃.
6.7 Centrifuge. ≥ 8000 r/min.
7 Quantitative analysis steps
7.1 Sample preparation
Mix the sample thoroughly before sampling, and take out 5.0 g~10.0 g sample.
Note. viscous samples should be shaken sufficiently to ensure uniform mixing.
7.2 Extraction
Weigh 1.0 g of the above sample, accurate to 0.01 g, add it to the centrifuge tube (6.3), add 10 mL directly to the weighed sample
Methanol (5.1), seal and shake and mix, ultrasonically extract at (60 ± 1) ℃ for 30 min, centrifuge and transfer the supernatant extract to 25 mL
Volumetric flask (6.5), add 10 mL of methanol (5.1) to the centrifuge tube (6.3) and shake well to wash, after centrifugation, transfer the supernatant for extraction
Fill it to the volumetric flask (6.5), and use methanol (5.1) to make the volume constant. Dilute the sample solution 4 times and transfer it to a sample bottle for liquid chromatography measurement.
7.3 Determination
7.3.1 Liquid chromatography conditions
Since the test results depend on the instrument used, it is impossible to give general parameters for liquid chromatography analysis. The set parameters shall be guaranteed
SN/T 5244-2020
To prove that the measured component can be effectively separated from other components during chromatographic determination, the following parameters prove to be feasible.
a) Chromatographic column. C18 reverse phase column, Diamonsil C18 (2), 3.0 mm × 150 mm, 3 μm or equivalent 1).
b) Column temperature. 35 ℃.
c) Mobile phase A. methanol; mobile phase B. acetonitrile; mobile phase C. water. See Table 1 for gradient elution.
d) Fluorescence detector. excitation wavelength 230 nm, emission wavelength 296 nm.
e) Flow rate. 0.50 mL/min.
f) Injection volume. 10 μL.
7.3.2 Liquid chromatography determination
The standard solution (5.9) and the sample solution are interspersed with equal volumes, and the standard solution and the sample solution to be tested contain alkylphenol and alkylphenol polyoxyethylene
The response value of the enether should be within the linear range of the standard solution, otherwise it needs to be diluted to a suitable concentration before measurement. The color of the sample to be tested
The deviation between the retention time of the peak and the retention time of the corresponding chromatographic peak of the standard solution is within ±2.5%, and the external standard method is used according to the area of the chromatographic peak
Quantitative.
Analyze the standard solution (5.9) according to the above analysis conditions (7.3.1), and the obtained alkylphenol and alkylphenol polyoxyethylene
See Appendix A for the liquid chromatogram of ether.
7.4 Confirmation of results
7.4.1 Confirmation conditions
The sample solution and standard solution with a positive result detected in 7.3.2 are carried out by the following two or one of the following liquid chromatographic separation and analysis methods
Confirmation of the retention time comparison of the detected substance, the deviation of the retention time between the chromatographic peak of the detected substance and the chromatographic peak of the corresponding standard solution
Within ±2.5%, it can be regarded as the same substance.
Since the test results depend on the instrument used, it is impossible to give general parameters for liquid chromatography analysis. The set parameters shall be guaranteed
Prove that the measured component can be effectively separated from other components during chromatographic determination. The parameters given below prove to be feasible.
7.4.2 Confirmation method of C8 column
C8 column analysis conditions include.
a) Chromatographic column. C8 reverse phase column, Diamonsil C8 (2), 3.0 mm × 150 mm, 3 μm or equivalent
1).
b) Chromatographic column temperature. 35 ℃.
c) Mobile phase A. methanol; mobile phase B. acetonitrile; mobile phase C. water. See Table 2 for gradient elution.
1) It is an example of a suitable commercially available product. This information is given for the convenience of users of this standard, and does not mean approval of this product. If other equivalent products have
With the same effect, these equivalent products can be used.
SN/T 5244-2020
d) Fluorescence detector. excitation wavelength. 230 nm; emission wavelength. 296 nm.
e) Flow rate. 0.45 mL/min.
f) Injection volume. 10 μL.
7.4.3 Confirmation method of phenyl chromatographic column
The analysis conditions of phenyl chromatographic column include.
a) Chromatographic column. phenyl column, Inertsil Ph-3, 3.0 mm × 150 mm, 3 μm or equivalent 2).
b) Chromatographic column temperature. 35 ℃.
c) Mobile phase A. methanol; mobile phase B. acetonitrile; mobile phase C. water. See Table 3 for gradient elution.
d) Fluorescence detector. excitation wavelength. 230 nm; emission wavelength. 296 nm.
e) Flow rate. 0.50 mL/min.
f) Injection volume. 10 μL.
7.5 Blank test
Except that no sample is added, the above determination steps (7.2-7.3) are carried out.
7.6 Result calculation
Calculate the content of alkylphenol and alkylphenol polyoxyethylene ether in the sample according to formula (1).
2) It is an example of a suitable commercially available product. This information is given for the convenience of users of this standard, and does not mean approval of this product. If other equivalent products have
With the same effect, these equivalent products can be used.
X--The content of alkyl phenol or alkyl phenol polyoxyethylene ether in the sample, in milligrams per kilogram (mg/kg);
Ai--the chromatographic peak area value of alkyl phenol or alkyl phenol polyoxyethylene ether in the sample extract;
A0--the chromatographic peak area value of alkyl phenol or alkyl phenol polyoxyethylene ether in blank sample;
cs--The concentration of alkyl phenol or alkyl phenol polyoxyethylene ether in the standard working solution, in milligrams per liter (mg/L);
V--The final constant volume of the sample solution, in milliliters (mL);
As--the chromatographic peak area value of alkyl phenol or alkyl phenol polyoxyethylene ether in standard working solution;
m--The sample volume represented by the final sample solution, in grams (g).
7.7 Presentation of results
The calculation of the test result is accurate to one decimal place, and the rounding of the value shall be carried out in accordance with the provisions of GB/T 8170.
8 Low detection limit and recovery rate
8.1 Lower limit of determination
Methods The detection limit of octylphenol, nonylphenol, octylphenol polyoxyethylene ether and nonylphenol polyoxyethylene ether in samples
10 mg/kg.
8.2 Recovery rate
The method recovery rate is 80% ~ 120%.
9 Test report
The test report should include at least the following.
a) Use the method of this standard;
b) Information of the sample;
c) Sample pretreatment record;
d) Measured results of all APnEO or part of APnEO in the sample;
e) Abnormal phenomena during the test;
f) Test date.
Appendix A
(Informative appendix)
Liquid chromatograms of alkyl phenol and alkyl phenol polyoxyethylene ether standards
...
