GB/T 23322-2018Textiles - Determination of surfactant - Alkylphenols and alkylphenol ethoxylates (English PDF)

4.3 Acetonitrile (HPLC grade).

4.4 n-hexane (HPLC grade).

4.5 Isopropanol (HPLC grade).

4.6 Dichloromethane (HPLC grade).

4.7 Methanol-aqueous solution (3 + 2): Accurately take 300 mL of methanol (4.2) and 200 mL of water. Mix well. Prepare for later use.

4.8 Methanol-dichloromethane solution (1 + 4): Accurately take 100 mL of methanol (4.2) and 400 mL of dichloromethane (4.6). Mix well. Prepare for later use.

4.10 Nonylphenol standard (NP, CAS No.25154-52-3, excellent grade pure).

4.11 Standard product of octylphenol ethoxylates (OPnEO, CAS No.9002-93-1, average degree of polymerization n = 9, excellent grade pure).

4.12 Standard product of nonylphenol ethoxylates (NPnEO, CAS No.9016-45-9, average degree of polymerization n = 9, purity ≥ 99%).

4.13 Standard stock solution: Accurately weigh an appropriate amount of OP (4.9), NP (4.10), OPnEO (4.11), NPnEO (4.12), respectively. Use methanol, to prepare a singlecomponent standard stock solution, which has a concentration of 10 mg/mL.

4.14 Standard working solution: Pipette an appropriate volume of OP, NP, OPnEO, NPnEO standard stock solution (4.13), respectively. Place in the same volumetric flask. Use methanol to dilute it. Prepare a mixed standard working solution of the required concentration.

4.15 Solid phase extraction column: The filler is lipophilic divinylbenzene and hydrophilic N-vinylpyrrolidone copolymer, 60 mg, 3 mL. Use 2 mL of methanol and 4 mL of water, to activate it in sequence, before use.

4.16 Organic filter membrane: 0.22 μm.

5.1 Liquid chromatography-mass spectrometer: Equipped with an electrospray

5.2 Analytical balance: Sensitivity is 0.0001 g.

5.3 Analytical balance: Sensitivity is 0.01 g.

5.4 Ultrasonic cleaner: The temperature can be controlled at (70 ± 2) °C.

5.5 Rotary evaporator.

5.6 Solid phase extraction device.

6.1 Extraction and purification of specimens

Take a representative specimen. Cut it into pieces of about 5 mm × 5 mm. Mix well. Weigh 1 g of the cut specimen (accurate to 0.01 g). Place it in a 50 mL centrifuge tube. Add 30 mL of methanol. Extract ultrasonically at (70 ± 2) °C, for (60 ± 5) min. Concentrate the extract to near dryness, at below 40 °C, by a rotary evaporator. Add 2 mL of methanol accurately, to dissolve the residue. Pass it through a 0.22 µm filter membrane (4.16). Use it for liquid chromatography-mass spectrometry determination.

When impurities in the specimen (such as silk) interfere with the detection, the following purification methods are used. Use 10 mL of methanol-water solution (4.7), to dissolve the residue in the above concentration bottle. Transfer all to the solid phase extraction column (4.15). Control the flow rate, to be 1 mL/min ~ 2 mL/min. Discard the effluent. Empty it under reduced pressure, for 10 min. Use 5 mL of methanoldichloromethane solution (4.8) to elute it. Collect the eluate. Use nitrogen, to blow dry the eluent below 40 °C. Add 2 mL of methanol accurately, to dissolve the residue. Pass it through a 0.22 µm filter membrane (4.16). Then use it for liquid chromatographymass spectrometry determination.

6.2 Determination

Since the test results depend on the instrument used, it is impossible to give general parameters for chromatographic analysis. The following parameters have been shown to be suitable for testing: 2) Mobile phase: AP analysis mobile phase is methanol-water-acetonitrile (19 + 75 + 6), isocratic elution; APnEO gradient elution conditions are as shown in Table 1; 1) Ion source: Electrospray ion source; […]

6.2.3 Qualitative determination

7.1 Calculation formula of LC-MS method

Calculate the content of alkylphenols and alkylphenol ethoxylates in the specimen, according to formula (1):

X - The content of the analyte in the specimen, in milligrams per kilogram (mg/kg);

c - The concentration of the analyte in the sample solution, which is obtained from the standard working curve, in milligrams per liter (mg/L);

c0 - The concentration of the analyte in the blank test solution, which is obtained from the standard working curve, in milligrams per liter (mg/L);

V - The final constant volume of the sample solution, in milliliters (mL);

m - The mass of the specimen, which is represented by the final sample solution, in grams (g).

The result is rounded off to two decimal places.

7.2 Calculation formula of LC-MS/MS method

Calculate the mass fraction of each component, in APnEO, according to formula (2):

Rn - The mass fraction of APnEO, which has a degree of aggregation of n;

An - The peak area of APnEO, which has a degree of aggregation of n;

ΣAi - Sum of APnEO peak area (degree of polymerization from 2 ~ 16).

Calculate the concentration of APnEO, which has a degree of polymerization of n, in the standard working solution, according to formula (3):

Cn - The concentration of APnEO, which has a degree of polymerization n, in the standard working solution, in milligrams per liter (mg/L);

Rn - The mass fraction of APnEO, which has a degree of polymerization n;

Cs - The concentration of APnEO standard working solution, in milligrams per liter (mg/L).

8.2 Recovery rate

The range of recovery rate of the method is 80% ~ 110%.

8.3 Precision

In the same laboratory, when the same operator uses the same equipment and the same test method, to independently test the same tested object, in a short period of time, the absolute difference, between the two independent test results, is not greater than 10% of the arithmetic mean of the two measured values. […]

A.1 Overview

This Appendix gives the method for the determination of alkylphenol (AP) and alkylphenol ethoxylates (APnEO, n = 2 ~ 16) in textiles, by reversed-phase high performance liquid chromatography.

A.2 Principle

The AP and APnEO in the specimen are extracted ultrasonically by methanol. After the extract is concentrated and purified, it is determined by a high performance liquid chromatograph, which is equipped with a fluorescence detector; then quantified by the external standard method.

A.3 Reagents or materials

A.4 Instruments and equipment

A.4.1 High performance liquid chromatograph, which is equipped with fluorescence detector.

A.4.3 Analytical balance: The sensitivity is 0.01 g.

A.4.5 Rotary evaporator.

A.4.6 Solid phase extraction device.

A.4.7 Nitrogen blower.

A.5 Determination steps

A.5.1 Extraction and purification of specimen

Take a representative specimen. Cut it into pieces of about 5 mm × 5 mm. Mix well. Weigh 1 g of the cut specimen (accurate to 0.01 g). Place it in a 50 mL centrifuge tube. Add 30 mL of methanol. Extract ultrasonically at (70 ± 2) °C, for (60 ± 5) min. Concentrate the extract to near dryness, at below 40 °C, by a rotary evaporator. Add 2 mL of methanol accurately, to dissolve the residue. Pass it through a 0.22 µm filter membrane (4.16). Use it for reversed phase liquid chromatography determination. When impurities in the specimen (such as silk) interfere with the detection, the following purification methods are used. Use 10 mL of methanol-water solution (4.7), to dissolve the residue in the above concentration bottle. Transfer all to the solid phase extraction column (4.15). Control the flow rate, to be 1 mL/min ~ 2 mL/min. Discard the effluent. Empty it under reduced pressure, for 10 min. Use 5 mL of methanoldichloromethane solution (4.8) to elute it. Collect the eluate. Use nitrogen, to blow dry the eluent below 40 °C. Add 2 mL of methanol accurately, to dissolve the residue. […]

A.5.2 Determination

B.1 Overview

This Appendix gives the normal phase high performance liquid chromatography method, for the determination of alkylphenol (AP) and alkylphenol ethoxylates (APnEO, n = 2 ~ 16), in textiles.

B.2 Principle

The AP and APnEO in the specimen are extracted ultrasonically by methanol. […]

B.3 Reagents or materials

B.3.1 Unless otherwise specified, the reagents used in this method are all analytically pure; the water is the grade-1 water, which is specified in GB/T 6682.

B.3.2 Methanol (HPLC grade).

B.3.3 Acetonitrile (HPLC grade).

B.3.4 n-hexane (HPLC grade).

B.3.5 Isopropanol (HPLC grade).

B.3.16 Organic filter membrane: 0.22 μm.

B.4 Instruments and equipment

B.4.1 High performance liquid chromatograph, which is equipped with fluorescence detector.

B.4.3 Analytical balance: The sensitivity is 0.01 g.

B.4.5 Rotary evaporator.

B.4.6 Solid phase extraction device.

B.4.7 Nitrogen blower.

B.5 Determination steps

B.5.1 Extraction and purification of specimens

Take a representative specimen. Cut it into pieces of about 5 mm × 5 mm. Mix well. Weigh 1 g of the cut specimen (accurate to 0.01 g). Place it in a 50 mL centrifuge tube. Add 30 mL of methanol. Extract ultrasonically at (70 ± 2) °C, for (60 ± 5) min. Concentrate the extract to near dryness, at below 40 °C, by a rotary evaporator. Add 2 mL of isopropanol accurately, to dissolve the residue. Pass it through a 0.22 µm filter membrane (B.3.16). Use it for normal phase high performance liquid chromatography determination. When impurities in the specimen (such as silk) interfere with the detection, the following purification methods are used. Use 10 mL of methanol-water solution (B.3.7), to dissolve the residue in the above concentration bottle. Transfer all to the solid phase extraction column (B.3.15). Control the flow rate, to be 1 mL/min ~ 2 mL/min. Discard the effluent. Empty it under reduced pressure, for 10 min. Use 5 mL of methanoldichloromethane solution (B.3.8) to elute it. Collect the eluate. Use nitrogen, to blow dry the eluent below 40 °C. Add 2 mL of isopropanol accurately, to dissolve the residue. […]

B.5.2 Determination

B.8 Test report

C.2 Principle

The AP and APnEO in the specimen are extracted ultrasonically by methanol. After the extract is concentrated and purified, it is determined by a high performance liquid chromatograph, which is equipped with a fluorescence detector; quantified by the external standard method.

C.3 Reagents or materials

C.3.1 Unless otherwise specified, the reagents used in this method are all analytically pure; the water is the grade-1 water, which is specified in GB/T 6682.

C.3.2 Methanol (HPLC grade).

C.3.3 Acetonitrile (HPLC grade).

C.3.4 n-hexane (HPLC grade).

C.3.5 Isopropanol (HPLC grade).

C.3.6 Dichloromethane (HPLC grade).

C.3.7 Methanol-water solution (3 + 2): Accurately measure 300 mL of methanol (C.3.2) and 200 mL of water. Mix well. Prepare for later use. C.3.8 Methanol-dichloromethane solution (1 + 4): Accurately measure 100 mL of methanol (C.3.2) and 400 mL of dichloromethane (C.3.6). Mix well. Prepare for later use. C.3.10 Nonylphenol standard (NP, CAS No.25154-52-3, excellent grade pure). C.3.11 Standard product of octylphenol ethoxylates (OPnEO, CAS No.9002-93-1, average degree of polymerization n = 9, excellent grade pure). C.3.12 Standard product of nonylphenol ethoxylates (NPnEO, CAS No.9016-45-9, average degree of polymerization n = 9, purity ≥ 99%). C.3. […]

C.4 Instruments and equipment

C.4.1 High performance liquid chromatograph, which is equipped with fluorescence detector.

C.4.2 Analytical balance: Sensitivity is 0.0001 g.

C.4.3 Analytical balance: Sensitivity is 0.01 g.

C.4.5 Rotary evaporator.

C.4.6 Solid phase extraction device.

C.5 Determination steps

C.5.1 Extraction and purification of specimens

Take a representative specimen. Cut it into pieces of about 5 mm × 5 mm. Mix well. Weigh 1 g of the cut specimen (accurate to 0.01 g). Place it in a 50 mL centrifuge tube. Add 30 mL of methanol. Extract ultrasonically at (70 ± 2) °C, for (60 ± 5) min. Concentrate the extract to near dryness, at below 40 °C, by a rotary evaporator. Add 2 mL of acetonitrile accurately, to dissolve the residue. Pass it through a 0.22 µm filter Time / min Acetonitrile / % Water / % membrane (C.3.16). […]

C.5.2 Determination

C.8 Test report