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Paper, board and paper products - Determination of alkylphenol polyethoxylates - HPLC-MS method
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GB/T 39998-2021
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Basic data | Standard ID | GB/T 39998-2021 (GB/T39998-2021) | | Description (Translated English) | Paper, board and paper products - Determination of alkylphenol polyethoxylates - HPLC-MS method | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | Y30 | | Word Count Estimation | 9,985 | | Issuing agency(ies) | State Administration for Market Regulation, China National Standardization Administration |
GB/T 39998-2021: Paper, board and paper products - Determination of alkylphenol polyethoxylates - HPLC-MS method ---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.
Paper, board and paper products-Determination of alkylphenol polyethoxylates-HPLC-MS method
ICS 85.010
Y30
National Standards of People's Republic of China
Paper, cardboard and paper products
Determination of alkylphenol polyoxyethylene ethers
High performance liquid chromatography mass spectrometry
Released on 2021-04-30
2021-11-01 implementation
State Administration of Market Supervision and Administration
Issued by the National Standardization Management Committee
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
Please note that some of the contents of this document may involve patents. The issuing agency of this document is not responsible for identifying these patents.
This standard was proposed by the China National Light Industry Council.
This standard is under the jurisdiction of the National Paper Industry Standardization Technical Committee (SAC/TC141).
Drafting organizations of this standard. Shanghai Institute of Quality Supervision and Inspection Technology, China Pulp and Paper Research Institute Co., Ltd., Hefei Schindler Packaging
Co., Ltd., Zhejiang Sanyang Packaging Industry Co., Ltd.
The main drafters of this standard. Zhao Lei, Zuo Ying, Yang Jianping, Tai Dongfang, Lang Yuanfeng, Luo Chan, Li Wenhui, Chen Zhongli, Chen Jingru.
Paper, cardboard and paper products
Determination of alkylphenol polyoxyethylene ethers
High performance liquid chromatography mass spectrometry
Warning---Personnel using this standard should have practical experience in formal laboratory work. This standard does not point out all possible safety issues
question. 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 standard specifies the determination method of alkylphenol polyoxyethylene ether content in paper, paperboard and paper products---high performance liquid chromatography
Spectrum method.
This standard applies to the determination of the content of octylphenol polyoxyethylene ether and nonylphenol polyoxyethylene ether in paper, paperboard and paper products.
It can also be used as a reference.
In this standard, the detection limit of octylphenol polyoxyethylene ether and nonylphenol polyoxyethylene ether is 0.3mg/kg, and the limit of quantification is both
1.0mg/kg.
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
3 Principle
After the crushed sample is extracted by methanol ultrasonic, the extract is transferred to a volumetric flask to constant volume. After the solution is filtered by the filter membrane, use high-performance liquid
The content of octylphenol polyoxyethylene ether and nonylphenol polyoxyethylene ether was determined by a chromatographic mass spectrometer. Use ESI positive mode detection,
Quantification by external standard method.
4 Reagents and materials
4.1 Water, GB/T 6682, level one.
4.2 Methanol (CH3OH). chromatographically pure.
4.3 10mmol/L ammonium acetate (CH3COONH4) solution. Weigh 0.77g ammonium acetate (chromatographically pure), add 1000mL water (4.1) to dissolve
Solve and mix well.
4.4 Octylphenol polyoxyethylene ether (OPEs) standard product (average degree of polymerization n=9~10), CAS number 9002-93-1, purity ≥95%.
4.5 Nonylphenol polyoxyethylene ethers (NPEOs) standard products (average degree of polymerization n=9~10), CAS number 9016-45-9, purity ≥95%.
4.6 Organic filter membrane (or filter). 0.22μm.
5 Equipment
5.1 High performance liquid chromatography mass spectrometer. equipped with an electrospray ion source (ESI).
5.2 Ultrasonic constant temperature water bath.
5.3 Analytical balance. Sensitivity is 0.0001g.
5.4 Crusher. speed 8000r/min~10000r/min.
5.5 Constant temperature drying oven. The temperature can be controlled at (50±2)℃.
5.6 Conventional laboratory glassware.
6 Preparation of Standards
6.1 Standard stock solution of octylphenol polyoxyethylene ether (1000mg/L). accurately weigh 0.1g (accurate to 0.1mg) of octylphenol polyoxyethylene
The standard ethyl ether (4.4) was diluted with methanol (4.2) in a 100mL volumetric flask to a constant volume and mixed. The solution is stored at 4℃, the expiration date
6 months.
6.2 Nonylphenol polyoxyethylene ether standard stock solution (1000mg/L). accurately weigh 0.1g (accurate to 0.1mg) nonylphenol polyoxyethylene
The standard ethyl ether (4.5) was diluted with methanol (4.2) in a 100mL volumetric flask to a constant volume and mixed. The solution is stored at 4℃, the expiration date
6 months.
6.3 Mixed standard intermediate solution (10mg/L). Pipette octylphenol polyoxyethylene ether standard stock solution (6.1) and nonylphenol polyoxyethylene respectively
Enether standard stock solution (6.2) 1.0mL each in a 100mL volumetric flask, dilute to volume with methanol, and mix.
6.4 Preparation of standard curve working solution. accurately pipette 0.05mL, 0.10mL, 0.20mL, 0.30mL, 0.50mL mixed standards respectively
The solution is placed in a 10mL volumetric flask with methanol to a constant volume and prepared as 0.05mg/L, 0.10mg/L, 0.20mg/L, 0.30mg/L, 0.50mg/L
Series of standard solutions. The standard working curve can be adjusted according to the actual concentration of the sample to be tested.
7 Sample preparation
7.1 Paper and cardboard
Take at least 10g sample and cut it to pieces below 5mm×5mm. The cardboard can also be crushed by a crusher (5.4) to crush the sample into
Flocculent or fragments below 5mm.
7.2 Paper products
7.2.1 Samples that are not easy to cut
For diapers (sheets, pads) and sanitary napkins (pads) and other samples that are not easy to be cut and mixed, at least one complete sample should be taken and a crusher should be used
(5.4) After crushing into flocculent shape, weigh the sample after mixing. The final sampling mass is not less than 10g.
7.2.2 Wipes
For wet wipes, in order to ensure uniform sampling, take one each from the upper, middle and lower parts of the two packs of wet wipes, and accurately weigh the total mass of 6 wet wipes m1
(Accurate to 0.1mg), placed on a clean aluminum box or watch glass, put the container with the sample in a constant temperature drying oven (5.5), at 50 ℃
Dry in a constant temperature drying box for 3 hours. In order to ensure that the sample is dried as soon as possible, the sample can be placed in multiple containers, and the sample should be avoided as much as possible. quasi-
Weigh the total mass of the dried sample m2 (accurate to 0.1mg), cut it to pieces below 1cm×1cm, and mix them.
8 Analysis steps
8.1 Extraction
Weigh 2g of the prepared sample (accurate to 0.1mg) into a 40mL sample bottle or Erlenmeyer flask, add 20mL methanol (4.2),
Ultrasonic constant temperature water bath (5.2), ultrasonic treatment at room temperature for 30min. Then transfer the sample extract, and use 20 mL of methanol for the residue
Repeat the extraction once, combine the extraction solutions in a 50mL volumetric flask, and dilute to the mark with methanol. Filtered by 0.22μm filter membrane (4.6),
Measured by high performance liquid chromatography mass spectrometer (5.1).
8.2 Determination
8.2.1 Reference conditions for high performance liquid chromatography
The reference conditions of HPLC are as follows.
a) Chromatographic column. C18, 50mm×3.0mm, inner diameter 2.7μm, or equivalent;
b) Mobile phase. methanol. 10mmol/L ammonium acetate solution (4.3)=80.20;
c) Flow rate. 0.4mL/min;
d) Column temperature. 35℃;
e) Injection volume. 5μL.
8.2.2 Reference conditions for mass spectrometry
The mass spectrometry reference conditions are as follows.
a) Ionization method. cation electrospray ionization source (ESI);
b) Ion scan mode. Scan (qualitative), SIM (quantitative);
c) Capillary voltage. 3500V;
d) Nozzle voltage. 500V;
e) Drying gas temperature. 325℃;
f) Dry air flow. 7L/min;
g) Atomizing gas pressure. 0.31MPa (45psi);
h) Sheath gas temperature. 325℃;
i) Sheath gas flow. 10L/min;
j) Monitoring ion range. m/z=150~1500.
8.2.3 Qualitative and quantitative analysis of high performance liquid chromatography mass spectrometry
8.2.3.1 Qualitative analysis
Analyze the standard curve working solution (6.4) and the sample solution to be tested according to the analysis conditions of 8.2.1 and 8.2.2.
The retention time and the characteristic qualitative ions of alkyl phenol polyoxyethylene ether (see Appendix A) are used for qualitative analysis. In the actual measurement process of the sample,
It is necessary to use Scan (scan ion range m/z=150~1500), that is, the mass spectrum of the sample should contain the characteristic ion of [M NH4]
A series of adduct ion peaks of the ions, these adduct ion peaks present a certain normal distribution, and each adduct ion peak has a difference in adjacent masses
44.It can be determined that the compound is an alkylphenol polyoxyethylene ether, and other means can be used to confirm if necessary.
8.2.3.2 Quantitative analysis
Inject the standard curve working solution (6.4) and the sample solution to be tested into the high performance liquid chromatography mass spectrometer (5.1),
(Or NPEOs) concentration is the abscissa, OPEs (or NPEOs) characteristic ion (see Appendix A) mass chromatographic peak area is the ordinate, plotted
Standard working curve.
Obtain the concentration of OPEs (or NPEOs) in the sample solution to be tested according to the standard working curve. If the concentration exceeds the standard working curve
Scope, it can be analyzed after diluting with methanol to an appropriate concentration.
Refer to Appendix B for the total ion chromatogram and mass spectrum of alkylphenol polyoxyethylene ether liquid chromatography mass spectrometry.
8.3 Blank test
Except for no samples, proceed in accordance with 8.1 and 8.2.
9 Result calculation
9.1 Calculation of alkylphenol polyoxyethylene ether content in wet tissue samples
Calculate the content of alkylphenol polyoxyethylene ether in wet wipes according to formula (1).
Xi=
(c1-c0)×V×f×m2
m×m1
(1)
Where.
Xi ---The content of alkylphenol polyoxyethylene ether in the sample, in milligrams per kilogram (mg/kg);
c1 --- The concentration of the alkylphenol polyoxyethylene ether corresponding to the sample solution in the standard curve, in milligrams per liter (mg/L);
c0 --- The concentration of alkylphenol polyoxyethylene ether corresponding to the blank solution in the standard curve, in milligrams per liter (mg/L);
V ---The constant volume of the sample, the unit is milliliters (mL);
f ---dilution factor;
m2---The total mass of 6 wet tissue samples after drying, in grams (g);
m --- sample sampling quality, the unit is grams (g);
m1 - The total mass of 6 wet tissue samples, in grams (g).
9.2 Calculation of alkylphenol polyoxyethylene ether content in other samples
Calculate the content of alkyl phenol polyoxyethylene ether according to formula (2).
Xi=
(c1-c0)×V×f
(2)
Where.
Xi ---The content of alkylphenol polyoxyethylene ether in the sample, in milligrams per kilogram (mg/kg);
c1 --- The concentration of the alkylphenol polyoxyethylene ether corresponding to the sample solution in the standard curve, in milligrams per liter (mg/L);
c0 --- The concentration of alkylphenol polyoxyethylene ether corresponding to the blank solution in the standard curve, in milligrams per liter (mg/L);
V ---The constant volume of the sample, the unit is milliliters (mL);
f ---dilution factor;
m --- sample sampling quality, the unit is grams (g).
10 Presentation of results
The calculation result is expressed as the arithmetic mean of two independent determination results obtained under repeated conditions, and the result retains three significant digits.
11 Precision
The absolute difference between two independent determination results obtained under repeated conditions shall not exceed 20% of the arithmetic mean.
12 Test report
The test report should include the following.
a) The number of this standard;
b) Test date and location;
c) Complete identification of all the information required for the sample;
d) Test results;
e) Any deviation from this standard;
f) Any operation method that affects the measurement result.
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