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GB/T 33285-2016 English PDF (GBT33285-2016)

GB/T 33285-2016 English PDF (GBT33285-2016)

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GB/T 33285-2016: Leather and fur -- Chemical tests -- Determination of nonylphenol and nonylphenol ethoxylates
GB/T 33285-2016
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 59.140.30
Y 46
Leather and fur - Chemical tests - Determination of
nonylphenol and nonylphenol ethoxylates
ISSUED ON: DECEMBER 13, 2016
IMPLEMENTED ON: JULY 01, 2017
Issued by: General Administration of Quality Supervision, Inspection and
Quarantine;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Normative references ... 4 
3 Principle ... 4 
4 Reagents and materials ... 5 
5 Instruments and devices ... 6 
6 Specimen preparation ... 6 
7 Analysis steps ... 7 
8 Result representation ... 10 
9 Test report ... 10 
Annex A (informative) Preparation of aluminum triiodide ... 12 
Annex B (informative) GC-MS chromatogram and mass spectrum of
nonylphenol ... 13 
Leather and fur - Chemical tests - Determination of
nonylphenol and nonylphenol ethoxylates
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
6.1 Sampling
6.1.1 Sampling on standard parts
Carry out for leather in accordance with the provisions of QB/T 2706. Carry out
for fur in accordance with the provisions of QB/T 1267. The sampling process
should avoid hair loss.
6.1.2 Sampling on non-standard parts
If it is not possible to sample from standard parts (such as shoes, clothing),
sampling shall be taken anywhere within the available area. The sample shall
Use 20mL of n-hexane (4.3) to extract twice. Combine the separated n-hexane
extracts. Add sodium thiosulfate solution (4.9) dropwise and shake until the
color of the solution disappears. The separated n-hexane is dehydrated by
anhydrous sodium sulfate (4.5). Conduct rotary evaporation to near dry.
Accurately add 2mL of n-hexane (4.3) to dissolve the residue. The solution is
filtered through the polyamide filter membrane (5.10) and then measured by
GC-MS to obtain nonylphenol chromatographic peak area, recorded as Ai2.
NOTE: In the test, please refer to Annex A to prepare an appropriate amount of aluminum
triiodide. Then directly add 10mL of specimen extract to it. Reflux for 10min at 90°C.
7.4 Test conditions of gas chromatography-mass spectrometry (GC-MS)
7.4.1 The gas chromatography (GC) conditions are as follows:
- Sampling system: splitless;
- Carrier gas: helium;
- Injection volume: 1μL;
- Capillary column: 30m×0.25mm (inner diameter) × 1μm (film thickness),
such as DB-5ms quartz capillary column;
- Gas flow: 1.0mL/min;
- Inlet temperature: 280°C;
- Chromatography mass spectrometer interface temperature: 250°C;
- Column temperature: 80°C for 1min, rise to 280°C at 10°C/min, for 10min.
7.4.2 Mass spectrometry (MS) conditions are as follows:
- Ionization method: EI;
- Ionization energy: 70eV;
- Test method: selected ion monitoring (SIM), m/z=107,121,135,149;
- Mass scanning range: (50~300) amu;
- Ion source temperature: 230°C;
- Quadrupole temperature: 150°C;
- Solvent delay: 5min.
7.5 Gas chromatography-mass spectrometry (GC-MS) determination
(mg/kg);
xNPEO - The content of nonylphenol ethoxylates in the sample, in milligrams per
kilogram (mg/kg);
V - The final constant volume of sample solution, in milliliters (mL);
m - The mass of the sample represented by the final sample volume, in grams
(g);
cs1 - The content of nonylphenol found from the standard curve, in milligrams
per liter (mg/L);
cs2 - The content of nonylphenol ethoxylates found from the standard curve, in
milligrams per liter (mg/L).
When calculating cs1, the chromatographic peak area obtained in the blank test
shall be deducted from Ai1. When calculating cs2, the chromatographic peak
area obtained from the blank test and the chromatographic peak area Ai1
obtained in 7.2 shall be deducted from Ai2.
7.9 Detection limit and recovery rate
The detection limits of this method for nonylphenol and nonylphenol ethoxylates
in samples are 1.0mg/kg and 3.0mg/kg, respectively. The recovery rate of the
method is between 80%~110%.
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;

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