GB/T 18414-2025 PDF EnglishUS$260.00 · In stock · Download in 9 seconds
GB/T 18414-2025: Textiles - Determination of chlorinated phenols and ortho-phenylphenol Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid GB/T 18414: Historical versions
Similar standardsGB/T 18414-2025: Textiles - Determination of chlorinated phenols and ortho-phenylphenol---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/GBT18414-2025GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 59.080.01 CCS W 04 Replacing GB/T 18414.1-2006, GB/T 18414.2-2006 and GB/T 20386-2006 Textiles - Determination of Chlorinated Phenols and Ortho- phenylphenol Issued on: FEBRUARY 28, 2025 Implemented on: MARCH 1, 2027 Issued by. State Administration for Market Regulation; Standardization Administration of the People’s Republic of China. Table of ContentsForeword... 3 1 Scope... 5 2 Normative References... 5 3 Terms and Definitions... 5 4 Principle... 5 5 Reagents and Materials... 5 6 Instruments and Equipment... 7 7 Specimen Preparation... 7 8 Test Steps... 7 9 Quantitation Limits, Recovery Rates and Precision... 9 10 Test Report... 9 Appendix A (normative) Basic Information of Chlorinated Phenols and Ortho- phenylphenol... 11 Appendix B (informative) Example of Gas Chromatography-Mass Spectrometry (GC- MS) Analysis Test Parameters... 12 Appendix C (informative) Total Ion Chromatogram of GC-MS Analysis of Acetylated Chlorinated Phenols and Ortho-phenylphenol Standard Substances / Standard Samples ... 15 Appendix D (informative) Spiked Recovery Rate of Negative Samples... 17 Textiles - Determination of Chlorinated Phenols and Ortho- phenylphenol WARNING. personnel using this document shall have practical experience in formal laboratory work. This document does not address all possible safety issues. The user is responsible for taking appropriate safety measures and ensuring compliance with the conditions stipulated by relevant national laws and regulations.1 ScopeThis document describes the determination method for 19 chlorinated phenols and ortho- phenylphenol in textiles by gas chromatograph-mass spectrometer (GC-MS). This document applies to all kinds of textile products.2 Normative ReferencesThe contents of the following documents constitute indispensable clauses of this document through the normative references in the text. In terms of references with a specified date, only versions with a specified date are applicable to this document. In terms of references without a specified date, the latest version (including all the modifications) is applicable to this document. GB/T 6682 Water for Analytical Laboratory Use - Specification and Test Methods3 Terms and DefinitionsThis document does not have terms or definitions that need to be defined.4 PrincipleAfter the specimen is ultrasonically extracted by potassium hydroxide / methanol solution, it is derivatized by acetic anhydride and extracted by n-hexane, and then, determined by gas chromatography-mass spectrometry using the internal standard method.5 Reagents and MaterialsUnless otherwise specified, all reagents used are of analytical grade. 5.1 n-Hexane. CAS No.. 110-54-3, chromatographically pure. 5.2 Water. Grade-3 water specified in GB/T 6682. 5.3 Acetic anhydride. CAS No.. 108-24-7. 5.4 Anhydrous sodium sulfate. CAS No.. 7757-82-6. 5.5 Chlorinated phenols and ortho-phenylphenol standard substances / standard samples. purity 97% (mass fraction), in accordance with the provisions of Appendix A. 5.6 2-Chlorophenol-d4 (internal standard 1). CAS No.. 93951-73-6, purity 97% (mass fraction). 5.7 2,4-Dichlorophenol-d3 (internal standard 2). CAS No.. 93951-74-7, purity 99% (mass fraction). 5.8 2,3,4,6-Tetrachlorophenol-13C6 (internal standard 3). CAS No.. 1246820-81-4, purity 98% (mass fraction). 5.9 Pentachlorophenol-13C6 (internal standard 4). CAS No.. 85380-74-1, purity 98% (mass fraction). 5.10 Potassium hydroxide solution. weigh-take an appropriate amount of potassium hydroxide and use water to prepare it into 2 mol/L potassium hydroxide solution. 5.11 Standard stock solution. respectively weigh-take appropriate amounts of chlorinated phenols and ortho-phenylphenol standard substances / standard samples (5.5) (accurate to 0.1 mg) and use acetonitrile (chromatographically pure) to prepare them into 1,000 mg/L stock solution. NOTE. the standard stock solution is stored in an environment of 0 C ~ 4 C and has a validity period of 6 months. 5.12 Mixed standard working solution. pipette an appropriate amount of the standard stock solution (5.11) of chlorinated phenols and ortho-phenylphenol and use potassium hydroxide solution (5.10) to prepare it into 10 mg/L mixed working solution. NOTE. the mixed standard working solution is stored in an environment of 0 C ~ 4 C and has a validity period of 1 month. 5.13 Internal standard stock solution. weigh-take an appropriate amount of the internal standard (5.6 ~ 5.9) (accurate to 0.1 mg) and use potassium hydroxide solution (5.10) to prepare it into 100 mg/L internal standard stock solution. NOTE. the internal standard stock solution is stored in an environment of 0 C ~ 4 C and has a validity period of 6 months. 5.14 Extraction solution. respectively pipette an appropriate amount of the internal standard stock solution (5.13), add an appropriate amount of methanol (chromatographically pure), and use potassium hydroxide solution (5.10) to prepare it into potassium hydroxide / methanol (volume ratio 1.1) extraction solution containing 10 g/L internal standard. 5.15 Organic phase needle filter. with a pore size of 0.45 m.6 Instruments and Equipment6.1 Gas chromatograph-mass spectrometer (GC-MS). equipped with electron impact ionization source (EI). 6.2 Analytical balance. respectively with an accuracy of 0.1 mg and 0.01 g. 6.3 Ultrasonic water bath generator. controllable temperature (70 5) C, operating frequency (40 5) kHz. 6.4 Vortex mixer. 6.5 Mechanical oscillator. the oscillation frequency is about 200 times/min (one reciprocating motion is 1 time), and the horizontal amplitude is 2 cm ~ 5 cm. 6.6 Pipette. 1 mL ~ 10 mL, 10 L ~ 100 L. 6.7 Extraction bottle. about 50 mL, made of hard glass, with a stopper.7 Specimen PreparationSelect a sufficient amount of representative sample, cut it into pieces with a maximum size not exceeding 5 mm, evenly mix them, and use an analytical balance (6.2) to accurately weigh-take 1.0 g (accurate to 0.01 g) from them as the specimen for later use.8 Test Steps8.1 Extraction Place the specimen prepared in 7 in an extraction bottle (6.7), add 20 mL of extraction solution (5.14), then, seal the stopper, and in an ultrasonic generator (6.3) in a (70 5) C water bath, extract it for 2 h 5 min. 8.2 Acetylation After the extraction is completed, take out the above-mentioned extraction bottle, cool it to room temperature, and add 2 mL of acetic anhydride (5.3). Use a vortex mixer (6.4) to vortex and oscillate it for 1 min, then, add 2.0 mL of n-hexane (5.1), use a mechanical oscillator (6.5) to mechanically oscillate it for 30 min at room temperature, and let it stand for stratification. Add an appropriate amount of anhydrous sodium sulfate (5.4), take part of the supernatant liquid and filter it through an organic phase needle filter (5.15) into a sampling bottle for GC- MS determination (8.4). 8.3 Acetylation of Standard Working Solution Use a pipette (6.6) to pipette a certain volume of the mixed standard working solution (5.12) into an extraction bottle (6.7), add 20 mL of extraction solution (5.14), and in accordance with the steps of 8.2, handle it. Prepare at least 5 concentrations of acetylated standard working solutions (such as. 0.02 mg/L, 0.05 mg/L, 0.2 mg/L, 0.5 mg/L and 1.0 mg/L). 8.4 Gas Chromatography-Mass Spectrometry 8.4.1 Analysis conditions Appendix B gives an example of gas chromatography-mass spectrometry (GC-MS) analysis test parameters. 8.4.2 Qualitative analysis Under the analysis conditions of 8.4.1, by comparing the retention time of the specimen solution with that of the standard working solution (the retention time deviation tolerance is 0.1 min), in addition, in the mass spectrum of the sample after background subtraction, the reference qualitative ions shall all appear, and the abundance ratio of the qualitative ions shall be consistent with the relative abundance ratio of the standard working solution with an equivalent concentration (see Appendix B), then, it can be determined that the corresponding analyte is present in the sample. The total ion chromatogram of GC-MS analysis of acetylated chlorinated phenols and ortho- phenylphenol standard substances / standard samples is shown in Appendix C. 8.4.3 Quantitative analysis In accordance with the content of the analyte in the specimen, select the standard working solution with similar response value and use the internal standard method for quantitative analysis. Take the ratio of the peak area of the target compound under the quantitative ion channel to the peak area of the corresponding internal standard as the vertical axis, and the ratio of the concentration of the target compound to the concentration of the corresponding internal standard as the horizontal axis to draw the standard working curve. The response values of the target substances in the specimen solution shall all be within the linear range of the instrument detection. If they exceed the range of the standard working curve, the specimen solution shall be diluted to an appropriate concentration before analysis. 8.5 Blank Test Except that no specimen is added, carry out the test in accordance with the steps 8.1 ~ 8.4. 8.6 Result Calculation In accordance with Formula (1), respectively calculate the contents of chlorinated phenols and ortho-phenylphenol. The calculation result shall retain two decimal places.Appendix B(informative) Example of Gas Chromatography-Mass Spectrometry (GC-MS) Analysis Test Parameters Since the test results depend on the instruments used, it is not possible to give general parameters for chromatographic analysis. The set parameters shall ensure that the component under test can be effectively separated from other components when determined under chromatographic conditions. The following parameters are proven to be feasible. a) Capillary chromatography column. DB-23, 30 m 0.25 mm 0.25 m or equivalent; b) Inlet temperature. 250 C; c) Heating program. initial temperature 50 C, maintain for 1 min, at 10 C/min, raise to 180 C, maintain for 1 min, then, at 12 C/min, raise to 240 C, maintain for 2 min; d) Ion source temperature. 230 C; e) Mass spectrometer interface temperature. 280 C; f) Determination mode. selected ion monitoring (SIM); selected ions are shown in Table B.1; g) Injection mode. splitless injection; h) Solvent delay time. 10.5 min; i) Carrier gas. helium 99.999% (volume fraction), flow rate 1.2 mL/min; j) Injection volume. 1.0 L; k) Ionization mode. EI; l) Ionization energy. 70 eV. ......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 18414-2025 be delivered?Answer: The full copy PDF of English version of GB/T 18414-2025 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 18414-2025_English with my colleagues?Answer: Yes. The purchased PDF of GB/T 18414-2025_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 18414-2025 -- 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.Question 5: Should I purchase the latest version GB/T 18414-2025?Answer: Yes. Unless special scenarios such as technical constraints or academic study, you should always prioritize to purchase the latest version GB/T 18414-2025 even if the enforcement date is in future. Complying with the latest version means that, by default, it also complies with all the earlier versions, technically.How to buy and download a true PDF of English version of GB/T 18414-2025?A step-by-step guide to download PDF of GB/T 18414-2025_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 18414-2025". 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 |
