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Delivery: <= 8 days. True-PDF full-copy in English will be manually translated and delivered via email. GB/T 4949-2018: Chemical analysis methods for sacrificial anodes of Al-Zn-In system alloy Status: Valid GB/T 4949: Historical versions
Basic dataStandard ID: GB/T 4949-2018 (GB/T4949-2018)Description (Translated English): Chemical analysis methods for sacrificial anodes of Al-Zn-In system alloy Sector / Industry: National Standard (Recommended) Classification of Chinese Standard: H12 Classification of International Standard: 77.120.10 Word Count Estimation: 46,431 Date of Issue: 2018-05-14 Date of Implementation: 2018-12-01 Older Standard (superseded by this standard): GB/T 4949-2007 Regulation (derived from): National Standards Announcement No. 6 of 2018 Issuing agency(ies): State Administration for Market Regulation, China National Standardization Administration GB/T 4949-2018: Chemical analysis methods for sacrificial anodes of Al-Zn-In system alloy---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.Chemical analysis methods for sacrificial anodes of Al-Zn-In system alloy ICS 77.120.10 H12 National Standards of People's Republic of China Replace GB/T 4949-2007 Aluminum-zinc-indium alloy sacrificial anode chemical analysis method Published on.2018-05-14 2018-12-01 implementation State market supervision and administration China National Standardization Administration issued ContentForeword I 1 Scope 1 2 Normative references 1 3 Determination of zinc content by titration of ethylenediaminetetraacetic acid (Na2EDTA), square wave polarography and flame atomic absorption spectrometry4 Determination of indium content by flame atomic absorption spectrometry and square wave polarography5 Determination of cadmium by flame atomic absorption spectrometry and square wave polarography 10 Determination of tin content by 6-catechol violet-cetyltrimethylammonium bromide micelle solubilization spectrophotometry and square wave polarography 7 Determination of magnesium content by flame atomic absorption spectrometry and disodium edetate (Na2EDTA) titration 8 Determination of silicon content by ammonium oxalate-ferrous ammonium sulfate silicon molybdenum blue photometric method 9 Determination of titanium by diantipyrylmethane spectrophotometry 24 Determination of iron content by 10 phenanthroline spectrophotometry and flame atomic absorption spectrometry 11 Flame atomic absorption spectrometry and sodium diethyldithiocarbamate-trichloromethane extraction spectrophotometric determination of copper content 30 12 Determination of lead by graphite furnace atomic absorption spectrometry and square wave polarography 33 13 Determination of zinc, indium, cadmium, tin, magnesium, silicon, titanium, iron, copper and lead by inductively coupled plasma atomic emission spectrometry 37 14 Quality Assurance and Control 43 15 Test report 43ForewordThis standard was drafted in accordance with the rules given in GB/T 1.1-2009. This standard replaces GB/T 4949-2007 "Aluminum-Zinc-Indium Alloy Sacrificial Anode Chemical Analysis Method", and GB/T 4949-2007 The main technical changes are as follows. --- Expanded the scope of analysis of each element (see Chapter 1); ---Modified the purity of the aluminum matrix used for the calibration curve drawing (see 3.2.5.4, 3.3.5.5, 4.1.5.5, 4.2.5.5, 5.1.5.5, 5.2.5.5, 6.2.5.5, 7.1.5.5, 8.4.5, 10.2.5.5, 11.1.5.5, 12.1.5.5, 12.2.5.5), modified from pure specimens containing no elements to be tested Aluminum as a substrate; --- Revised the requirements for instrument performance in the flame atomic absorption method (see 3.3.3.2, 4.1.3.2, 5.1.3.2, 7.1.3.2, 10.2.3.2 11.1.3.2), the requirement of the detection limit in the flame atomic absorption spectrometer is changed to the sensitivity requirement, and the precision requirement is modified; --- Revised the amount of sample and the concentration of tin standard solution in the spectrophotometric method of tin, the amount of sample is changed from 0.1g to 0.5g (see 6.1.4.1), plus The concentration of the tin standard solution changed from 1 mg/mL to 0.005 mg/mL (see 6.1.4.5.1); --- Modified the number of digits after the calculation result is expressed to the decimal point (see 6.1.5, 6.2.6, 9.5, etc.); --- Revised the test report (see Chapter 15); --- Increased inductively coupled plasma atomic emission spectrometry for the determination of zinc, indium, cadmium, tin, magnesium, silicon, titanium, iron, copper and lead (see section 13 chapter); --- Increased quality assurance and control (see Chapter 14); ---Adjusted the order of analysis elements, and analyzed the analysis of zinc, magnesium, cadmium, indium, tin, lead, silicon, iron, copper and titanium in GB/T 4949-2007 The order is in accordance with the order of the elements in the chemical composition requirements of the aluminum-zinc-indium alloy sacrificial anode product standard (GB/T 4948). Adjustment. This standard was proposed by the National Marine Ship Standardization Technical Committee (SAC/TC12). This standard is sub-technical committee of marine materials application technology of the National Marine Ship Standardization Technical Committee (SAC/TC12/SC4) Return to the mouth. This standard was drafted. The 725th Research Institute of China Shipbuilding Industry Corporation. The main drafters of this standard. Du Mifang, Wang Hongfeng, Liu Pan, Du Lili, Yan Cunguo, Nie Fuqiang, Zhang Binbin, Li Jingbin, Tong Xiaohong, Gao Xia. The previous versions issued by this standard are as follows. ---GB/T 4949-1985, GB/T 4949-2007. Aluminum-zinc-indium alloy sacrificial anode chemical analysis method1 ScopeThis standard specifies the determination method of zinc, indium, cadmium, tin, magnesium, silicon, titanium, iron, copper and lead in the sacrificial anode of aluminum-zinc-indium alloy. This standard applies to the determination of zinc, indium, cadmium, tin, magnesium, silicon, titanium, iron, copper and lead in the sacrificial anode of aluminum-zinc-indium alloy. Elements The measurement range is shown in Table 1. Table 1 Measurement range of each element element Measuring range (mass fraction) Titration method square wave polarography photometric atomic absorption spectrometry inductively coupled plasma atomic emission spectrometry Zinc 1.00~8.00 1.00~5.00 - 1.00~5.00 1.00~10.00 Indium - 0.010~0.050 - 0.010~0.050 0.010~0.100 Cadmium - 0.0050~0.030 - 0.0050~0.030 0.0010~0.100 Tin - 0.010~0.050 0.010~0.050 - 0.010~0.100 Magnesium 0.500~4.00 - - 0.500~4.00 0.100~2.00 Silicon - - 0.020~0.200 - 0.010~0.300 Titanium - - 0.0050~0.100 - 0.0010~0.100 Iron - - 0.020~0.200 0.020~0.200 0.010~0.300 Copper - - 0.0010~0.020 0.0010~0.020 0.0010~0.050 Lead - 0.0010~0.0100 - 0.0010~0.0100 0.0010~0.01002 Normative referencesThe following documents are indispensable for the application of this document. For dated references, only dated versions apply to this article. Pieces. For undated references, the latest edition (including all amendments) applies to this document. GB/T 4948 aluminum-zinc-indium alloy sacrificial anode GB/T 6682-2008 Analytical laboratory water specifications and test methods GB/T 8170 Numerical Rounding Rules and Representation and Determination of Limit Values 3 Determination of zinc content by disodium edetate (Na2EDTA) titration, square wave polarography and flame atomic absorption spectrometry 3.1 Ethylenediaminetetraacetic acid disodium (Na2EDTA) titration 3.1.1 Principle After the sample was dissolved in hydrochloric acid and hydrogen peroxide, zinc (II) was complexed with thiocyanate in hydrochloric acid medium and quantified by 4-methyl-2-pentanone. Extraction, extraction with hexamethylenetetramine buffer solution to make zinc (II) into the aqueous phase, titrimetrically titrated with disodium edetate (Na2EDTA) Solution titration. 3.1.2 Reagents 3.1.2.1 Unless otherwise stated, only analytically pure reagents and distilled or deionized water or equivalent purity of water are used in the analysis. The water for analysis should at least meet the requirements for secondary water in GB/T 6682-2008. 3.1.2.2 Hydrochloric acid (ρ=1.19g/mL). 3.1.2.3 Hydrogen peroxide (ρ=1.11g/mL). 3.1.2.4 4-methyl-2-pentanone (ρ=0.80 g/mL). 3.1.2.5 Hydrochloric acid (1 1). 3.1.2.6 Thiourea solution (20g/L). 3.1.2.7 Ammonium thiocyanate solution (500g/L). 3.1.2.8 Ammonium fluoride solution (50g/L), stored in plastic bottles. 3.1.2.9 Ammonium thiocyanate solution (50g/L). Take 50mL ammonium thiocyanate solution (3.1.2.7), add 10mL hydrochloric acid (3.1.2.5), dilute with water Release to 500mL and mix. 3.1.2.10 Hexamethylenetetramine buffer solution (pH 5.8). Weigh 100g of hexamethylenetetramine, dissolve in water and transfer to 500mL volumetric flask Add 20 mL of hydrochloric acid (3.1.2.2), dilute to the mark with water, and mix. 3.1.2.11 Zinc standard solution (0.01500mol/L). Weigh 0.4903g pure zinc (the mass fraction of zinc is not less than 99.99%) in.200mL In the beaker, add a total amount of 40 mL of hydrochloric acid (3.1.2.5) in two portions. When the reaction is slow, dissolve by heating, dissolve completely, and then cool to room temperature. Transfer to a 500 mL volumetric flask, dilute to the mark with water, and mix. 3.1.2.12 Ethylenediaminetetraacetic acid disodium (Na2EDTA) standard titration solution, the preparation steps are as follows. a) Preparation. Weigh 3.72g of Na2EDTA, dissolve in water, transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix. b) Calibration. Pipette 15.00mL zinc standard solution (3.1.2.11) into a 250mL Erlenmeyer flask, add about 30mL water and 20mL six times Methyltetramine buffer solution (3.1.2.10), add 1 drop ~ 2 drops of xylenol orange solution (3.1.2.13), titrated with Na2EDTA standard Solution [3.1.2.12.a)] titrate until the color of the test solution changes from purple to pure yellow as the end point. Record consumption of Na2EDTA standard drops Determine the volume of the solution. c) Calculation. Calculate the concentration of the Na2EDTA standard titration solution according to formula (1). c= c0V1 V2 (1) In the formula. c --- Na2EDTA standard titration solution concentration in moles per liter (mol/L); C0 --- zinc standard solution concentration, in moles per liter (mol/L); V1---The volume of the zinc standard solution is taken in milliliters (mL); V2---The volume of the Na2EDTA standard titration solution consumed by the calibration zinc standard solution, in milliliters (mL). Take 3 parts for calibration, the difference of the volume of zinc standard titration solution consumed should not exceed 0.10mL, take the average value, otherwise, heavy New calibration. 3.1.2.13 xylenol orange solution (2g/L). 3.1.3 Sample Drill or pick up the specimen according to the provisions of GB/T 4948, the thickness of the specimen shall be no more than 1mm. 3.1.4 Analysis steps 3.1.4.1 Samples Weigh 1.00 g of the sample to the nearest 0.1 mg. 3.1.4.2 Number of measurements The measurement was performed twice independently, and the average value was taken. 3.1.4.3 Determination 3.1.4.3.1 Place the sample (3.1.4.1) in a.200mL Erlenmeyer flask and slowly add 20mL hydrochloric acid (3.1.2.5). When the reaction is slow, add Heat, add about 1 mL of hydrogen peroxide (3.1.2.3), heat and dissolve completely, and boil to decompose excess hydrogen peroxide. Cool to room temperature and move in In a 100 mL volumetric flask, dilute to the mark with water and mix. 3.1.4.3.2 Pipette 20.00mL of test solution (3.1.4.3.1) into a 250mL separatory funnel, and then add 5mL of thiourea solution (3.1.2.6), 50mL water, 10mL ammonium thiocyanate solution (3.1.2.7), shake well, add 20mL 4-methyl-2-pentanone (3.1.2.4), shake for 2min, let stand After stratification, the water phase is discarded. 3.1.4.3.3 Add 15mL ammonium thiocyanate solution (3.1.2.9) and 5mL ammonium fluoride solution (3.1.2.8) to the organic phase, shake for 1min, static After layering, the water phase is discarded. Repeat 1 time. 3.1.4.3.4 Add 20 mL of hexamethylenetetramine buffer solution (3.1.2.10) and 50 mL of water to the organic phase, shake for 1 min, and let stand for stratification. After that, the aqueous phase was placed in a 250 mL Erlenmeyer flask. 3.1.4.3.5 Add 15 mL of hexamethylenetetramine buffer solution (3.1.2.10) and 20 mL of water to the organic phase, shake for 1 min, and let stand for stratification. Thereafter, the aqueous phase was incorporated into a 250 mL Erlenmeyer flask. Repeat 1 time. 3.1.4.3.6 In the conical flask solution (3.1.4.3.5) add 1 drop ~ 2 drops of xylenol orange solution (3.1.2.13), titrate the solution with Na2EDTA standard (3.1.2.12) Titration until the color of the test solution changes from purple to pure yellow as the end point. The volume of the Na2EDTA standard titration solution was recorded. 3.1.5 Calculation and representation of analysis results The mass fraction of zinc, w(Zn), is calculated according to formula (2), and the value is expressed in %. w(Zn)= cVV0M m0V3×1000× 100 (2) In the formula. c --- Na2EDTA standard titration solution concentration in moles per liter (mol/L); V --- volume of Na2EDTA standard titration solution consumed by titration, in milliliters (mL); V0---the total volume of the test solution, the unit is milliliter (mL); The molar mass of M--zinc, in grams per mole (g/mol) (M = 65.39); M0---the mass of the sample, the unit is gram (g); V3---The volume of the test solution is taken in milliliters (mL). The result of the calculation is expressed as 2 digits after the decimal point. Digital rounding is carried out in accordance with the entry rules given in GB/T 8170. 3.2 Square wave polarography 3.2.1 Principle After the sample is dissolved by hydrochloric acid and hydrogen peroxide, in the ammoniacal ammonium chloride solution, the zinc ion produces a good reduction wave, and a large amount of aluminum is lemon. The acid salt was complexed, and the square wave polar wave height of the zinc square wave was measured by a square wave polarograph. 3.2.2 Reagents 3.2.2.1 Unless otherwise stated, only analytically pure reagents and distilled or deionized water or water of comparable purity are used in the analysis. The water for analysis should at least meet the requirements for secondary water in GB/T 6682-2008. 3.2.2.2 Ammonium chloride. 3.2.2.3 Sodium citrate. 3.2.2.4 anhydrous sodium sulfite. 3.2.2.5 Pure aluminum (the mass fraction of aluminum is not less than 99.99% or the mass fraction of zinc is not more than 0.00010%). 3.2.2.6 Hydrogen peroxide (ρ=1.11g/mL). 3.2.2.7 Ammonia (ρ=0.90g/mL). 3.2.2.8 Hydrochloric acid (ρ=1.19g/mL). 3.2.2.9 Hydrochloric acid (1 1). 3.2.2.10 Gelatin solution (1g/L). 3.2.2.11 Zinc standard solution (1mg/mL). Weigh 0.5000g of pure zinc (the mass fraction of zinc is not less than 99.99%) in a.200mL beaker In the middle, a total of 40mL of hydrochloric acid (3.2.2.9) is added in two portions. When the reaction is slow, it is dissolved by heating. After the dissolution is completed, it is cooled to room temperature and moved. Into a 500mL volumetric flask, dilute to the mark with water, and mix. 3.2.2.12 Methyl red ethanol solution (1g/L). 3.2.3 Instruments The square wave polarograph uses a mercury drop electrode as the cathode and a calomel electrode as the reference electrode. 3.2.4 Sample Drill or pick up the specimen according to the provisions of GB/T 4948, the thickness of the specimen shall be no more than 1mm. 3.2.5 Analysis steps 3.2.5.1 Samples Weigh 0.10 g of sample to the nearest 0.1 mg. 3.2.5.2 Number of measurements The measurement was performed twice independently, and the average value was taken. 3.2.5.3 Determination 3.2.5.3.1 Place the sample (3.2.5.1) in a 150 mL Erlenmeyer flask and add 10 mL of hydrochloric acid (3.2.2.9). When the reaction is slow, add 5 drops~ 10 drops of hydrogen peroxide (3.2.2.6), after heating and dissolved completely, boiled to decompose excess hydrogen peroxide. Cool to room temperature and transfer to 100mL capacity In the bottle, add 5g ammonium chloride (3.2.2.2) and 3g sodium citrate (3.2.2.3), add 1 drop of methyl red ethanol solution (3.2.2.12), use ammonia water (3.2.2.7) Neutralization to red disappeared and excess 5mL, add 1g anhydrous sodium sulfite (3.2.2.4) and 1mL gelatin solution (3.2.2.10), Dilute the water to the mark and mix. 3.2.5.3.2 Take part of the test solution (3.2.5.3.1) in the polarographic electrolysis cup, with the mercury drop electrode as the cathode and the calomel electrode as the reference electrode. Between -1.1V~-1.7V, the zinc half-wave potential is -1.33V, and the appropriate instrument parameters are selected to record the square wave polarographic wave height of zinc. 3.2.5.3.3 Find the corresponding amount of zinc from the calibration curve in 3.2.5.4. 3.2.5.4 Drawing of the calibration curve Weigh 6 parts of 0.1000g of pure aluminum (3.2.2.5) and place them in 6 150mL conical flasks, adding 0mL and 1.00mL in sequence. 2.00mL, 3.00mL, 4.00mL, 5.00mL zinc standard solution (3.2.2.11), the following operation according to 3.2.5.3.1~3.2.5.3.2. respectively The wave height of the test solution without the zinc standard solution is deducted, and the calibration curve is drawn by taking the amount of zinc as the abscissa and the wave height as the ordinate. 3.2.6 Calculation and representation of analysis results The mass fraction of zinc, w(Zn), is calculated according to formula (3), and the value is expressed in %. w(Zn)= M1 M0×1000× 100 (3) In the formula. M1---the amount of zinc found in the calibration curve in milligrams (mg); M0---The mass of the sample in grams (g). The result of the calculation is expressed as 2 digits after the decimal point. Digital rounding is carried out in accordance with the entry rules given in GB/T 8170. 3.3 Flame atomic absorption spectrometry 3.3.1 Principle After the sample was dissolved in hydrochloric acid and hydrogen peroxide, it was measured by an air-acetylene lean flame at an atomic absorption spectrometer at a wavelength of 213.9 nm. The absorbance of zinc. 3.3.2 Reagents 3.3.2.1 Unless otherwise stated, only analytically pure reagents and distilled or deionized water or water of comparable purity are used in the analysis. The water for analysis should at least meet the requirements for secondary water in GB/T 6682-2008. 3.3.2.2 Pure aluminum (the mass fraction of aluminum is not less than 99.99% or the mass fraction of zinc is not more than 0.00010%). 3.3.2.3 Hydrogen peroxide (ρ=1.11g/mL). 3.3.2.4 Hydrochloric acid (ρ=1.19g/mL). 3.3.2.5 Hydrochloric acid (1 1). 3.3.2.6 Zinc standard solution (1mg/mL). Weigh 0.5000g of pure zinc (the mass fraction of zinc is not less than 99.99%) in a.200mL beaker In the middle, a total amount of 40 mL of hydrochloric acid (3.3.2.5) was added in two portions. When the reaction was slow, it was dissolved by heating. After the dissolution was completed, it was cooled to room temperature. Transfer to a 500 mL volumetric flask, dilute to the mark with water, and mix. 3.3.3 Instruments 3.3.3.1 Atomic absorption spectrometer with zinc hollow cathode lamp. 3.3.3.2 The instrument shall meet the following requirements. a) Sensitivity. The characteristic concentration of zinc should not exceed 0.02 μg/mL in the solution consistent with the measurement sample solution. b) Precision. The absorbance is measured 10 times with the highest concentration of the standard solution, and the standard deviation should not exceed 1.0% of the average absorbance; 10 absorbances are measured with the lowest concentration of standard solution (not a "zero concentration" solution), the standard deviation of which should not exceed the maximum concentration The standard solution has an average absorbance of 0.5%. c) Calibration curve characteristics. The calibration curve is divided into 5 segments according to the concentration, and the difference between the absorbance difference of the highest segment and the absorbance of the lowest segment is Ratio should be no less than 0.7. 3.3.4 Sample Drill or pick up the specimen according to the provisions of GB/T 4948, the thickness of the specimen shall be no more than 1mm. 3.3.5 Analysis steps 3.3.5.1 Samples Weigh 0.10 g of sample to the nearest 0.1 mg. 3.3.5.2 Number of tests The measurement was performed twice independently, and the average value was taken. ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB/T 4949-2018_English be delivered?Answer: Upon your order, we will start to translate GB/T 4949-2018_English as soon as possible, and keep you informed of the progress. The lead time is typically 5 ~ 8 working days. 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