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GB/T 4698.8-2017 PDF English

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GB/T 4698.8-2017: Methods for chemical analysis of titanium sponge, titanium and titanium alloys - Part 8: Determination of aluminum content - Separation with sodium hydroxide-EDTA complex-metric titration and inductively coupled plasma atomic emission spectrometry
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GB/T 4698.8: Evolution and historical versions

Standard IDContents [version]USDSTEP2[PDF] deliveryName of Chinese StandardStatus
GB/T 4698.8-2017English170 Add to Cart 0-9 seconds. Auto-delivery Methods for chemical analysis of titanium sponge, titanium and titanium alloys - Part 8: Determination of aluminum content - Separation with sodium hydroxide-EDTA complex-metric titration and inductively coupled plasma atomic emission spectrometry Valid
GB/T 4698.8-1996English159 Add to Cart 2 days Sponge titanium, titanium and titanium alloys. Determination of aluminum content. Separation with sodium hydroxide. EDTA complexometric titration method Obsolete
GB/T 4698.8-1984EnglishRFQ ASK 3 days Methods for chemical analysis of titanium and titanium alloys--The separation with sodium hydroxide--EDTA complexometric titration method for the determination of aluminum content Obsolete

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GB/T 4698.8-2017: Methods for chemical analysis of titanium sponge, titanium and titanium alloys - Part 8: Determination of aluminum content - Separation with sodium hydroxide-EDTA complex-metric titration and inductively coupled plasma atomic emission spectrometry



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GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 77.120.50 H 14 Replacing GB/T 4698.8-1996 Methods for chemical analysis of titanium sponge, titanium and titanium alloys - Part 8: Determination of aluminum content - Separation with sodium hydroxide - EDTA complex-metric titration and inductively coupled plasma atomic emission spectrometry ISSUED ON: SEPTEMBER 29, 2017 IMPLEMENTED ON: APRIL 01, 2018 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 ... 6 2 Method One - Alkali separation - EDTA complexometric titration ... 6 3 Method Two -- Inductively coupled plasma atomic emission spectrometry . 11 4 Test report ... 14 Methods for chemical analysis of titanium sponge, titanium and titanium alloys - Part 8: Determination of aluminum content - Separation with sodium hydroxide - EDTA complex-metric titration and inductively coupled plasma atomic emission spectrometry

1 Scope

This Part of GB/T 4698 specifies the methods to determine aluminum content in sponge titanium, titanium and titanium alloys. This Part is applicable to the determination of aluminum content in sponge titanium, titanium and titanium alloys. The determination range: 0.80%~8.50% for Method One; 0.010%~8.50% for Method Two. When the determination ranges overlap, Method One is the arbitration analysis method.

2 Method One - Alkali separation - EDTA

complexometric titration 2.1 Method summary The test material is dissolved with sulfuric acid. Separate the elements such as titanium, iron, chromium, zirconium, copper, manganese and part of vanadium by sodium hydroxide precipitation. In a weakly acidic medium of pH5, add EDTA complex aluminum. Use zinc acetate standard titration solution to titrate excessive EDTA. Add potassium fluoride to complex aluminum and release quantitative EDTA. Then use zinc acetate standard titration solution to titrate EDTA released, so as to obtain the aluminum content. For tin interference determination, add potassium iodide to volatilize to remove. Vanadium affects the judgment of the end point of titration. Add hydroxylamine hydrochloride to eliminate its interference. 2.2 Reagents Unless otherwise stated, only the confirmed analytically-pure reagents and laboratory grade two water are used in the analysis. 2.2.1 Nitric acid (ρ=1.42g/mL). 2.2.2 Sulfuric acid (1+1). 2.2.3 Hydrochloric acid (1+1). 2.2.4 Potassium iodide solution (200g/L). 2.2.5 Ferric chloride solution (50g/L): Weigh 5g of iron trichloride (FeCl3·6H2O) and dissolve it in 100mL of hydrochloric acid (1+99). 2.2.6 Sodium hydroxide solution (300g/L). 2.2.7 Sodium hydroxide solution (150g/L). 2.2.8 Copper chloride solution (10g/L): Weigh 1g of copper chloride (CuCl2·2H2O) and dissolve it in 100mL of water. 2.2.9 Hydroxylamine hydrochloride solution (100g/L). 2.2.10 Disodium ethylenediaminetetraacetic acid (Na2EDTA) solution [c(Na2EDTA)]=0.05mol/L]: Weigh 18.6g of Na2EDTA (C10H14N2O8Na2·2H2O) into a 500mL beaker. Add 300mL of water to dissolve. Transfer to a 1000mL volumetric flask. Use water to dilute to the scale mark. Mix well. 2.2.11 Hexamethylenetetramine buffer solution (pH5): Weigh 150g of hexamethylenetetramine in a 1000mL beaker. Add 400mL of water to dissolve. Add about 50mL of hydrochloric acid (ρ=1.19g/mL) to adjust the solution to about pH 5 (check with pH test paper). Use water to dilute to 500mL. Mix well. 2.2.12 Potassium fluoride solution (200g/L): Stored in plastic bottles. 2.2.13 Aluminum standard storage solution: Weigh 1.0000g of metallic aluminum (wAl≥99.99%) into a 300mL beaker. Add 20mL of sodium hydroxide solution (2.2.6). After the violent reaction stops, heat to dissolve. Remove it and cool. Add hydrochloric acid (2.2.3) until the precipitated precipitate is dissolved with an excess of 20mL. Cool. Transfer to a 1000mL volumetric flask. Use water to dilute to the scale mark. Mix well. 1mL of this solution contains 1.0mg of aluminum. 2.2.14 Standard titration solution of zinc acetate [c(Zn2+)≈0.014mol/L]. 2.2.14.1 Preparation: Weigh 3g of zinc acetate [Zn(CH3COO)2·2H2O] into a 200mL beaker. Add 50mL of water to dissolve. Add 2mL of glacial acetic acid (ρ=1.05g/mL). Transfer to a 1000mL volumetric flask. Use water to dilute to the scale mark. Mix well. 2.2.14.2 Calibration: Pipette three portions of 5.00mL of aluminum standard 3.2.3 Nitric acid (ρ=1.42g/mL). 3.2.4 Titanium (wTi≥99.9%, wAl< 0.005%). 3.2.5 Aluminum standard storage solution: Weigh 1.0000g of metallic aluminum (wAi≥99.99%) into a 300mL beaker. Add 20mL of sodium hydroxide solution (300g/L). After the violent reaction stops, heat to dissolve. Remove and cool. Add hydrochloric acid (3.2.1) until the precipitated precipitate is dissolved with an excess of 20mL. Cool. Transfer to a 1000mL volumetric flask. Use water to dilute to the scale mark. Mix well. 1mL of this solution contains 1mg of aluminum. 3.2.6 Aluminum standard solution A: Pipette 10.00mL of aluminum standard stock solution (3.2.5) into a 100mL volumetric flask. Add 5mL of hydrochloric acid (3.2.1). Use water to dilute to the scale mark. Mix well. 1mL of this solution contains 100μg of aluminum. 3.2.7 Aluminum standard solution B: Pipette 10.00mL of aluminum standard solution A (3.2.6) into a 100mL volumetric flask. Add 5mL of hydrochloric acid (3.2.1). Use water to dilute to the scale mark. Mix well. 1mL of this solution contains 10μg of aluminum. 3.2.8 Argon (volume fraction≥99.99%). 3.3 Instruments Inductively coupled plasma atomic emission spectrometer: Equipped with hydrofluoric acid resistant sampling system, of which the resolution is less than 0.006nm (at 200nm). 3.4 Specimen Follow the promulgated standards for sample preparation of sponge titanium, titanium and titanium alloys. 3.5 Analysis steps 3.5.1 Test material Weigh 0.10g of specimen (3.4), to the nearest of 0.0001g. 3.5.2 Number of determinations Conduct two determinations independently. Take the average value. 3.5.3 Blank test Conduct the blank test with test material. 3.5.4 Preparation of analytical test solution 3.5.4.1 Place the test material (3.5.1) in a 100mL PTFE beaker. Blow in a small amount of water. Add 5mL of hydrochloric acid (3.2.1). Add 1mL of hydrofluoric acid (3.2.2). Heat at low temperature until the sample is completely dissolved. Then add 0.5mL of nitric acid (3.2.3) dropwise until the solution is clear. Continue heating to drive off nitrogen oxides. Remove and cool to room temperature. 3.5.4.2 Transfer to a 100mL plastic volumetric flask. Use water to dilute to the scale mark. Mix well. 3.5.5 Preparation of working curve solution 3.5.5.1 Weigh 6 portions of titanium metal (3.2.4) equivalent to the titanium content of the test material (3.5.1) in a series of 100mL PTFE beakers. Operate according to 3.5.4.1 along with the test material. 3.5.5.2 Transfer the solution to six 100mL plastic volumetric flasks. Add 0mL, 1.00mL of aluminum standard solution B (3.2.7), 1.00mL of aluminum standard solution A (3.2.6), 1.00mL, 3.00mL, 6.00mL, 9.00mL of aluminum standard storage solution (3.2.5) in sequence. Use water to dilute to the scale mark. Mix well. 3.5.6 Measurement In the inductively coupled plasma atomic emission spectrometer, at the selected wavelength (the spectrum line is not specifically specified; the recommended analysis line wavelength of aluminum is 237.312nm, 394.401nm, and the interference of the spectrum line shall be checked when using it), determine the working curve solution (3.5.5.2). When the working curve is linear r≥0.999, conduct the determination of analysis test solution (3.5.4.2). Check the background of the element spectrum and correct it at the appropriate position. The mass concentration of aluminum element is automatically given by the computer. 3.6 Calculation of analysis results The amount of aluminum is calculated as the mass fraction of aluminum wAl, calculated according to formula (3): Where, ρ1 - The mass concentration of aluminum in the measured solution obtained from the working curve, in micrograms per milliliter (μg/mL); ......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.


      

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