GB/T 33285-2016 PDF EnglishUS$170.00 · In stock · Download in 9 seconds
GB/T 33285-2016: Leather and fur - Chemical tests - Determination of nonylphenol and nonylphenol ethoxylates Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Obsolete
Similar standardsGB/T 33285-2016: Leather and fur - Chemical tests - Determination of nonylphenol and nonylphenol ethoxylates---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT33285-2016 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 ContentsForeword ... 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 ethoxylates1 ScopeThis 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 referencesThe 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 samples3 PrincipleUse 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 devices5.1 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 preparation6.1 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 representationThe 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 reportThe 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; ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of English version of GB/T 33285-2016 be delivered?Answer: The full copy PDF of English version of GB/T 33285-2016 can be downloaded in 9 seconds, and it will also be emailed to you in 9 seconds (double mechanisms to ensure the delivery reliably), with PDF-invoice.Question 2: Can I share the purchased PDF of GB/T 33285-2016_English with my colleagues?Answer: Yes. The purchased PDF of GB/T 33285-2016_English will be deemed to be sold to your employer/organization who actually paid for it, including your colleagues and your employer's intranet.Question 3: Does the price include tax/VAT?Answer: Yes. Our tax invoice, downloaded/delivered in 9 seconds, includes all tax/VAT and complies with 100+ countries' tax regulations (tax exempted in 100+ countries) -- See Avoidance of Double Taxation Agreements (DTAs): List of DTAs signed between Singapore and 100+ countriesQuestion 4: Do you accept my currency other than USD?Answer: Yes. www.ChineseStandard.us -- GB/T 33285-2016 -- Click this link and select your country/currency to pay, the exact amount in your currency will be printed on the invoice. Full PDF will also be downloaded/emailed in 9 seconds.How to buy and download a true PDF of English version of GB/T 33285-2016?A step-by-step guide to download PDF of GB/T 33285-2016_EnglishStep 1: Visit website https://www.ChineseStandard.net (Pay in USD), or https://www.ChineseStandard.us (Pay in any currencies such as Euro, KRW, JPY, AUD).Step 2: Search keyword "GB/T 33285-2016". Step 3: Click "Add to Cart". If multiple PDFs are required, repeat steps 2 and 3 to add up to 12 PDFs to cart. Step 4: Select payment option (Via payment agents Stripe or PayPal). Step 5: Customize Tax Invoice -- Fill up your email etc. Step 6: Click "Checkout". Step 7: Make payment by credit card, PayPal, Google Pay etc. After the payment is completed and in 9 seconds, you will receive 2 emails attached with the purchased PDFs and PDF-invoice, respectively. Step 8: Optional -- Go to download PDF. Step 9: Optional -- Click Open/Download PDF to download PDFs and invoice. See screenshots for above steps: Steps 1~3 Steps 4~6 Step 7 Step 8 Step 9 |
