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Delivery: <= 4 days. True-PDF full-copy in English will be manually translated and delivered via email. GB/T 39994-2021: Determination of six metal elements (iron, calcium, magnesium, zinc, titanium, copper) in polyolefin pipe system Status: Valid
Basic dataStandard ID: GB/T 39994-2021 (GB/T39994-2021)Description (Translated English): Determination of six metal elements (iron, calcium, magnesium, zinc, titanium, copper) in polyolefin pipe system Sector / Industry: National Standard (Recommended) Classification of Chinese Standard: G33 Word Count Estimation: 18,147 Issuing agency(ies): State Administration for Market Regulation, China National Standardization Administration GB/T 39994-2021: Determination of six metal elements (iron, calcium, magnesium, zinc, titanium, copper) in polyolefin pipe system---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order. Determination of six metal elements (iron, calcium, magnesium, zinc, titanium, copper) in polyolefin pipe system ICS 83.140.30 CCSG33 National Standards of People's Republic of China Six metal elements in polyolefin pipelines (Iron, calcium, magnesium, zinc, titanium, copper) determination Released on 2021-04-30 2021-11-01 implementation State Administration of Market Supervision and Administration Issued by the National Standardization Management Committee Six metal elements in polyolefin pipelines (Iron, calcium, magnesium, zinc, titanium, copper) determination Warning---The method specified in this document requires the use of corrosive reagents. During operation, you should wear protective equipment, solution preparation and Sample pretreatment should be carried out in a fume hood. 1 ScopeThis document specifies the determination method for the six metals content of iron, calcium, magnesium, zinc, titanium and copper in polyolefin pipelines and raw materials. This document is applicable to the determination of the content of six metals (iron, calcium, magnesium, zinc, titanium, and copper) in various polyolefin pipes, fittings, and valves, as well as Determination of six metal elements (iron, calcium, magnesium, zinc, titanium, copper) in mixed ingredients, recycled materials and recycled materials (recycled materials).2 Normative referencesThe contents of the following documents constitute the indispensable clauses of this document through normative references in the text. Among them, dated quotations Only the version corresponding to that date is applicable to this document; for undated reference documents, the latest version (including all amendments) is applicable to This document. GB/T 602 Preparation of standard solutions for impurity determination of chemical reagents GB/T 6682-2008 Analytical laboratory water specifications and test methods GB/T 6819 dissolved acetylene GB/T 9345.1-2008 Determination of Ash in Plastics Part 1.General Method GB/T 19278-2018 General terms and definitions for thermoplastic pipes, fittings and valves GB/T 21187 Atomic Absorption Spectrophotometer GB/T 36244 Inductively coupled plasma atomic emission spectrometer GB/T 37837-2019 Quadrupole Inductively Coupled Plasma Mass Spectrometry Method General3 Terms and definitionsThe terms and definitions defined in GB/T 19278-2018 are applicable to this document.4 Method summaryAfter the sample is burned-dissolved or acid digested, the volume is constant, shaken, and the inductively coupled plasma emission spectrometer (ICP-OES), inductively coupled Plasma mass spectrometer (ICP-MS) and atomic absorption spectrometer (AAS) were used for measurement. Note. The choice of test equipment is related to the type and concentration of metal elements in the solution to be tested.5 Reagents or materials5.1 Concentrated nitric acid Analytical level and above. 5.2 Test water It complies with the 4.2 level 2 water regulations in GB/T 6682-2008. 5.3 Nitric acid solution with a volume fraction of 1% Add half the volume of test water (see 5.2) to a 100mL volumetric flask, then transfer 1.0mL of concentrated nitric acid (see 5.1), and wait to dissolve it. After the solution is cooled to room temperature, make the volume up to the mark with test water, and shake it for later use. 5.4 Single element standard solution [Iron (Fe), Calcium (Ca), Magnesium (Mg), Zinc (Zn), Titanium (Ti), Copper (Cu)] The single element standard solution can be prepared according to the regulations in GB/T 602, or it can be directly used with certified reference materials, and its mass concentration is 100mg/L~1000mg/L. 5.5 Multi-element standard solution [Iron (Fe), Calcium (Ca), Magnesium (Mg), Zinc (Zn), Titanium (Ti), Copper (Cu)] According to the mutual interference between the elements and the nature of the standard solution, it can be prepared in groups, or the certified standard substance can be used directly, and its mass concentration It is 100mg/L~1000mg/L. 5.6 Standard use solution Respectively pipet the standard solution (see 5.4 or 5.5) and dilute with nitric acid solution (see 5.3) to a constant volume. 5.7 Internal standard stock solution of inductively coupled plasma mass spectrometer Elements naturally present in samples, reagents or matrix cannot be used as internal standards; internal standard elements should not be subjected to isobaric or polyatomic ions. Disturbance can not interfere with the isotope of the measured element; the mass number of the internal standard element should be close to the mass number of the measured element. Recommended to choose Use 6Li, 45Sc, 74Ge, 89Y, 103Rh, 115In, 185Re, 209Bi as internal standard elements. You can prepare it yourself or purchase a certified standard solution directly. 5.8 Inductively coupled plasma mass spectrometer internal standard standard use solution Dilute the internal standard standard solution (see 5.7) with nitric acid (see 5.3) to prepare an internal standard standard solution. Due to the internal standard of different instruments in the pump tube Diameters are different, the concentration of the internal standard into the sampling system is different. It is recommended that the concentration of the internal standard solution after entering the sample is 5μg/L~50μg/L. 5.9 Mass spectrometry tuning solution for inductively coupled plasma mass spectrometer Different types of instruments have their own requirements for the types and concentrations of elements contained in the tuning solution. Prepare according to the instrument manual or directly purchase to meet the requirements. The required certified standard solution is prepared as a mass spectrometry tuning solution. 5.10 Argon The purity of argon is not less than 99.995% (volume fraction); acetylene should meet the requirements of GB/T 6819; it should be fully removed when using compressed air dust.6 Equipment6.1 Pretreatment equipment 6.1.1 Glassware All glassware should be soaked in nitric acid solution with a mass fraction of about 10% for at least 12h before use, and then washed with pure water for at least 4 times. 6.1.2 Quartz crucible For the quartz crucible with lid, the washing method is the same as 6.1.1. 6.1.3 Box-type resistance furnace The temperature can be controlled within the range of 850℃±50℃. 6.1.4 Electric heating plate The temperature is adjustable, and the working temperature should reach 500°C. Note. Other suitable heating sources can be used. 6.1.5 Microwave Digestion Apparatus The output power is 500W~2000W. With programmable control function, temperature and pressure can be monitored throughout the process, and with safety protection 6.1.6 Analytical balance The accuracy is 0.1mg. 6.2 Test equipment 6.2.1 Inductively coupled plasma emission spectrometer (ICP-OES) Should meet the requirements of GB/T 36244, the quartz cyclone atomization sampling system should be selected. 6.2.2 Inductively coupled plasma mass spectrometer (ICP-MS) It should meet the requirements of Chapter 6 of GB/T 37837-2019, and the quartz cyclone atomization sampling system should be used. 6.2.3 Atomic Absorption Spectrometer (AAS) Should meet the requirements of the flame atomic absorption spectrometer in GB/T 21187, and there is a hollow cathode lamp with the element to be measured.7 Sample preparation7.1 Sample cutting For pipes, fittings or valves, use a cutter to cut a clean sample larger than 10g, and then use scissors to cut into particles less than 5mm in length. use. The pellet sample can be used directly. If the detection target element is iron, titanium-coated scissors should be used when cutting into small particles to avoid cutting Introduce iron pollution, if the detection target element contains titanium element, you should use scissors that do not interfere with the verification target element. Note. The sampling amount of the sample is determined according to the metal element content in the sample and the detection capability of the equipment to meet the test requirements. 7.2 Sample preparation 7.2.1 General This document specifies two sample pretreatment methods. dry ashing method and microwave digestion method. 7.2.2 Dry ashing method Take double samples. The amount of sample taken should be enough to produce 5.0mg of ash. It is recommended that the initial sampling amount of the sample is about 10g. If it is enough to produce 5.0mg of ash, increase the sampling amount and re-process the sample. The specific steps are as follows. a) Burn the clean quartz crucible to constant weight in accordance with 5.3.1 of GB/T 9345.1-2008. b) Weigh an appropriate amount of sample, accurate to 0.1mg, and put it into a quartz crucible. c) Place the quartz crucible on the electric heating plate and heat it directly to slowly burn the sample until the sample forms a dry carbonized residue. only. The burning should not be too violent to avoid ash loss. If there are many samples, it needs to be burned in stages, and the amount added should not exceed quartz Half the height of the crucible. d) Put the quartz crucible containing the residue into the box-type high-temperature resistance furnace, and partially cover the quartz crucible lid to prevent ash loss. Burn at 850℃±50℃ for at least 30min to make the sample ashed completely. e) Remove the quartz crucible and lid from the furnace, put them in a desiccator, and allow them to cool to room temperature. f) Add an appropriate amount of nitric acid solution (see 5.3) to the quartz crucible, and oscillate the crucible in an ultrasonic oscillator for at least 1 min. After the element to be tested is completely dissolved, the solution is transferred to a volumetric flask, and the quartz crucible is washed three times with a small amount of nitric acid solution (see 5.3). The solution is added to the volumetric flask and the volume is made up to 25mL with nitric acid solution (see 5.3). g) After the fixed volume of the solution is filtered with a 0.45μm filter membrane, the sample solution to be tested is obtained. Note. When the ash content is higher, the dissolution may be incomplete. It is recommended to increase the constant volume. When the ash content is 5.0mg~50.0mg, 50.0mg~200.0mg, For.200.0mg~500.0mg, it is recommended to set the volume to 25mL, 50mL, and 100mL respectively. 7.2.3 Microwave Digestion Method The steps of the pre-treatment method for microwave digestion are as follows. a) Weigh two samples of 100.0mg~200.0mg (accurate to 0.1mg) into two digestion tanks, and add 4mL~ 6mL nitric acid (see 5.1) is pre-digested on an electric hot plate at 80℃~120℃ for 1h. b) Install the digestion tank according to the instructions of the microwave digestion instrument, and set the program (see Appendix A) for digestion. After the digestion process is over, the digestion tank should Cool to room temperature in the microwave digestion apparatus and take it out. c) Open the digestion tank cover in a fume hood, rinse the tank cover at least 3 times with a small amount of test water, and add the rinse solution to the digestion tank. Heat the acid on a hot plate at 120°C until the remaining solution volume is about 0.2 mL. d) Remove the digestion tank and cool it to 40℃~60℃, transfer the contents of the tank to a 25mL volumetric flask, and use nitric acid solution (see 5.3) Wash the inner wall of the digestion tank at least 3 times and transfer all the rinsing solution to a 25mL volumetric flask, and use nitric acid solution (see 5.3) to make the volume constant To the mark, shake well to obtain the sample solution to be tested. e) After filtering with a 0.45μm filter membrane, the sample solution to be tested is obtained. Note 1.The selection of digestion reagents can be adjusted according to the actual digestion situation. Hydrochloric acid, hydrofluoric acid, sulfuric acid, hydrogen peroxide and other reagents can be added to nitric acid to form a complex compound. Combine the digestion agent for digestion. The addition of hydrofluoric acid will cause corrosion to the sampling system of the instrument. It is recommended to choose the sampling system accessories that are resistant to hydrofluoric acid corrosion; The use of hydrogen oxide in the closed digestion process is dangerous. If the sample contains a large amount of easily oxidizable organic matter, avoid using it in the closed digestion process. Use hydrogen peroxide. Note 2.The amount of sample and the amount of digestion reagents are related to the type and size of the digestion tank used, and can be adjusted according to actual conditions. 7.3 Blank sample Without the sample, prepare the blank sample according to the same steps as the sample preparation (see 7.2.2 or 7.2.3).8 Test procedure8.1 Inductively coupled plasma spectrometer (ICP-OES method) 8.1.1 Preparation of standard working solution Use a pipette or pipette to pipette different volumes of standard use solution (see 5.6), and dilute with nitric acid solution (see 5.3) to obtain different Concentration of iron (Fe), calcium (Ca), magnesium (Mg), zinc (Zn), titanium (Ti), copper (Cu) standard working solution, the standard working solution has at least 5 concentrations The point and range are determined according to the metal element content of the sample to be tested. The blank standard working solution is nitric acid solution (see 5.3). 8.1.2 Drawing of calibration curve Start the inductively coupled plasma spectrometer. The recommended operating parameters are shown in Appendix B, B.1.After the equipment is stable, set the standard working solution (See 8.1.1) Pumped into the inductively coupled plasma emission spectrometer from low concentration to high concentration, taking the mass concentration of the target element as the abscissa, The emission intensity value is the ordinate, and the calibration curve of the target element is drawn. The correlation coefficient of the standard curve of the inductively coupled plasma spectrometer should be Greater than 0.999. Note 1.If spectral line overlap or spectral line interference occurs, other wavelengths can also be used. The wavelength should be selected to maintain sufficient sensitivity to achieve the necessary detection limit. Note 2.Because the working conditions of different ICP-OES instruments are different, the tester can determine the test parameters according to the instrument manual or test optimization. 8.1.3 Determination of blank sample Flush the sampling system with nitric acid solution (see 5.3) until the signal drops to a level close to that of the blank standard working solution, and then establish a calibration curve Analyze the blank sample under the same conditions (see 7.3). Make at least one blank sample for each batch of samples, and the blank value of the measured element shall not exceed the method The detection limit. If it exceeds, find out the reason and re-analyze the sample until it is qualified. 8.1.4 Determination of the solution to be tested Measure the solution to be tested according to the same operation steps as the blank sample determination (see 7.2), and according to the iron, calcium, magnesium, zinc, titanium, and titanium in the solution to be tested. Calculate the final content of the corresponding element in the sample with the concentration of copper element, the mass of the sample and the volume of the constant volume. If one or more elements in the solution to be tested If the concentration of is higher than the maximum concentration of the standard curve, use nitric acid (see 5.3) to dilute the test solution to the concentration range of the standard curve Re-measure. For every 10 samples analyzed, the midpoint concentration standard solution of a calibration curve is used for calibration verification. The relative deviation of the concentration at this point in the latest calibration curve should be ≤10%, otherwise the test data of the first 10 samples should be discarded and the calibration curve should be redrawn Then retest the first 10 samples. Note. X-ray fluorescence spectrometer can also be used to perform qualitative and semi-quantitative analysis of the element to be tested in the test sample in advance to estimate its approximate content to shorten the determination The time and process of whether the concentration of the element to be tested is within the calibration curve range. 8.2 Inductively coupled plasma mass spectrometry method (ICP-MS method) 8.2.1 Preparation of standard working solution Proceed as per 8.1.1. 8.2.2 Drawing of calibration curve Start the inductively coupled plasma mass spectrometer, when the vacuum degree of the instrument reaches the requirement, ignite the plasma and stabilize for 15-20min. After the instrument is stable, use the inductively coupled plasma mass spectrometer mass spectrometer tuning solution (see 5.9) to tune the various indicators of the instrument. After the indicators such as degree, oxide, double charge, resolution, etc. meet the instrument manual or measurement requirements, edit the measurement method (see B.2 for recommended working parameters). Note. For elements such as iron and magnesium, there are different degrees of polyatomic ion interference. This document recommends to select the collision mode to eliminate the same mass/connection to the greatest extent. Near polyatomic ion interference, other elements can choose standard mode or collision mode depending on the matrix and coexisting elements. Different types of instruments work The conditions are different, and the typical working parameters of the equipment are shown in Appendix B. After the instrument is stable, pump the standard working solution (see 8.2.1) from low concentration to high concentration sequentially into the inductively coupled plasma mass spectrometer instrument. The internal standard element standard solution (see 5.7) can be directly added to the standard working solution (see 8.2.1) and the solution to be tested, or it can be passed through Dynamic pump and three-way valve are added online. Take the mass concentration of the target element as the abscissa, and the mass spectrum peak height or peak area of the target element as the ordinate, draw The calibration curve of the target element. The correlation coefficient of the standard curve of the inductively coupled plasma mass spectrometer should be greater than 0.999. 8.2.3 Determination of blank samples Flush the sampling system with nitric acid solution (see 5.3) until the signal drops to a level close to that of the blank standard working solution, and then establish a calibration curve Analyze the blank sample under the same conditions (see 7.3). Make at least one blank sample for each batch of samples, and the blank value of the measured element shall not exceed the method The detection limit. If it exceeds, you must find the reason, re-analyze the sample until it is qualified. 8.2.4 Determination of the solution to be tested Measure the solution to be tested according to the same procedure as the blank sample measurement (see 7.2). During the test of the solution to be tested, the internal standard element should be monitored The intensity change of the element, the response value of the internal standard element should be between 70%~130% of the response value of the calibration curve when the sample is ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB/T 39994-2021_English be delivered?Answer: Upon your order, we will start to translate GB/T 39994-2021_English as soon as possible, and keep you informed of the progress. The lead time is typically 2 ~ 4 working days. 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