GB/T 33285-2016Leather and fur - Chemical tests - Determination of nonylphenol and nonylphenol ethoxylates (English PDF)

1 Scope

This Standard specifies the determination method - gas chromatography-mass spectrometry (GC-MS) for the contents of nonylphenol and nonylphenol ethoxylates in leather and fur. This Standard is applicable to the determination for octylphenol and octylphenol polyoxyethylene ether content in leather and fur.

This Standard is applicable to various leathers, furs and their products.

2 Normative references

The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.

GB/T 6682, Water for analytical laboratory use - Specification and test methods

QB/T 1267, Fur - Chemical, physical and mechanical and fastness tests -

Sampling location

QB/T 1272, Leather - Chemical tests - Preparation of chemical test samples

QB/T 2706, Leather - Chemical physical and mechanical and fastness tests

- Sampling location

QB/T 2716, Leather - Preparation of chemical test samples

3 Principle

Use acetonitrile as solvent. Use ultrasonic extraction method to extract the target in the sample. After the nonylphenol in the extract is extracted and separated by n-hexane, use gas chromatography-mass spectrometer (GC-MS) to test. The nonylphenol polyoxyethylene ether in the extract is first chemically converted into nonylphenol. Then test the separated nonylphenol by gas chromatography-mass spectrometry (GC-MS). Use its peak area as the basis product (4.7). Use acetonitrile (4.2) to prepare a standard stock solution with a concentration of 1mg/mL. Then as needed, use acetonitrile (4.2) to dilute to a working solution with a concentration in the range of 2mg/L~30mg/L.

NOTE: The standard stock solution can be stored in the refrigerator at 0°C~4°C for 12 months. The standard working solution can be stored in the refrigerator at 0°C~4°C and the validity period is 1 month.

5 Instruments and devices

5.1 Analytical balance: division value is 0.1mg.

5.2 Stoppered conical flask: 100mL.

5.3 Ultrasonic generator: frequency is 40kHz.

5.4 Oil bath or other suitable heaters: accuracy is ±1°C.

5.5 Pipettes: 2mL, 10mL, 50mL single-label pipettes or graduated pipettes.

5.6 Flat-bottomed flask: ground mouth, 50mL.

5.7 Separatory funnel: 150mL.

5.8 Glass fiber filter: GF8 or glass filter G3, diameter is 70mm~100mm.

5.9 Vacuum rotary evaporator.

5.10 Polyamide filter membrane: 0.45µm.

5.11 Gas chromatograph (GC): equipped with mass selector (MS).

6 Specimen preparation

8 Result representation

The relative deviation of the two parallel determination results shall be less than

10%. The content of nonylphenol and nonylphenol ethoxylates in the sample is expressed as the arithmetic mean of the results of two parallel tests, in mg/kg.

The result is kept to one decimal place.

9 Test report

The test report shall include the following:

a) Reference to this Standard;

b) Sample name, type, sampling details;

c) Content of nonylphenol and nonylphenol ethoxylates in the sample;

d) Abnormal phenomena during the test;

......