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GB/T 4698.2-2011 English PDF (GBT4698.2-2011)

GB/T 4698.2-2011 English PDF (GBT4698.2-2011)

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GB/T 4698.2-2011: Methods for chemical analysis of titanium sponge, titanium and titanium alloys -- Determination of iron content

This Part specifies the method for the measurement of iron content in sponge titanium, titanium, titanium alloys. This Part applies to the measurement of iron content, in sponge titanium, titanium, titanium alloys.
GB/T 4698.2-2011
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
ICS 77.120.50
H 64
Replacing GB/T 4698.2-1996
Methods for chemical analysis of titanium sponge, titanium
and titanium alloys - Measurement of iron content
ISSUED ON: MAY 12, 2011
IMPLEMENTED ON: FEBRUARY 01, 2012
Issued by: General Administration of Quality Supervision, Inspection and Quarantine of PRC;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative references ... 5
3 General ... 5
4 Method 1 -- 1,10-phenanthroline spectrophotometry ... 6
5 Method 2 -- Atomic absorption spectrometry ... 9
6 Method 3 -- Inductively coupled plasma atomic emission spectrometry ... 14 Appendix A (Informative) The structural changes of this Part, as compared with ISO 22960:2008, ISO 22961:2008, ISO 22962:2008 ... 22
Appendix B (Informative) Technical differences between method 1 of this Part and ISO 22960:2008, method 2 and ISO 22961:2008, method 3 and ISO 22962:2008 and their reasons ... 24
Methods for chemical analysis of titanium sponge, titanium
and titanium alloys - Measurement of iron content
1 Scope
This Part specifies the method for the measurement of iron content in sponge titanium, titanium, titanium alloys.
This Part applies to the measurement of iron content, in sponge titanium, titanium, titanium alloys.
2 Normative references
The following documents are essential to the application of this document. For the dated documents, only the versions with the dates indicated are applicable to this document; for the undated documents, only the latest version (including all the amendments) is applicable to this standard.
GB/T 6682 Water for analytical laboratory use - Specification and test methods (ISO 3696, MOD)
GB/T 12806 Laboratory glassware - One-mark volumetric flasks (ISO 1042, EQV) GB/T 12808 Laboratory glassware - One mark pipette (ISO 648, EQV)
GB/T 12809 Laboratory glassware - Principles of design and construction of volumetric glassware (ISO 384, EQV)
GB/T 12810 Laboratory glassware - Volumetric glassware - Methods for use and testing of capacity (ISO 4787, IDT)
3 General
3.1 Unless otherwise stated, only confirmed analytical pure reagents are used in the analysis; the water used is distilled water or deionized water or water of equivalent purity, which shall comply with the provisions of GB/T 6682.
3.2 The instruments used shall be within the calibration period. Their performance shall meet the technical parameters, which are required by the calibration. The glass containers shall be grade A, which is specified in GB/T 12808, GB/T 12809, GB/T 12806; the specific use method shall refer to the requirements of GB/T 12810. 4 Method 1 -- 1,10-phenanthroline spectrophotometry
4.1 Measurement range
The measurement range of iron is 0.005% ~ 2.00% (mass fraction).
4.2 Method principle
The sample is dissolved by hydrochloric acid-hydrofluoric acid. The titanium oxide nitric acid is added. The boric acid, tartaric acid, ammonium acetate, hydroxylamine hydrochloride is added. The 1,10-phenanthroline is added, to form 1,10-phenanthroline iron complex; the iron content is measured by spectrophotometer.
4.3 Reagents
4.3.1 Hydrochloric acid (1 + 1): Slowly add 500 mL of hydrochloric acid (??1.16 g/mL ~ 1.19 g/mL), into 500 mL water.
4.3.2 Nitric acid (1 + 1): Slowly add 500 mL of nitric acid (??1.42 g/mL), into 500 mL of water.
4.3.3 Hydrofluoric acid (1 + 1): Carefully and slowly add 100 mL of hydrofluoric acid (??1.14 g/mL), into 100 mL of water.
4.3.4 Boric acid.
4.3.5 Tartaric acid (200 g/L).
4.3.6 Ammonium acetate (500 g/L).
4.3.7 Hydroxylamine hydrochloride solution (100 g/L).
4.3.8 The 1,10-phenanthroline solution (2 g/L): Dissolve 2.0 g of 1,10-phenanthroline in 100 mL of ethanol (volume percentage not less than 95%). Use water to dilute it to 1000 mL.
4.3.9 Iron standard solution
4.3.9.1 Iron standard storage solution (0.500 mg/mL): Accurately weigh 0.500 g of metallic iron (wFe ??? 99.9%), into a 300 mL beaker (accurate to 0.0001 g). Add 30 mL of hydrochloric acid (4.3.1). Heat to dissolve it. Add 5 mL of nitric acid (4.3.2), to oxidize iron. Continue to heat, to drive off nitrogen oxides. Cool it down. Transfer to a 1000 mL volumetric flask. Use water to dilute it to the mark. Mix well. 4.3.9.2 Iron standard solution (0.050 mg/mL): Pipette 10.00 mL of iron standard stock solution (4.3.9.1), into a 100 mL volumetric flask. Use water to dilute it to the mark. 5.3.4 Boric acid.
5.3.5 Pure titanium
wTi ??? 99.95%; the iron content is known AND shall be as low as possible. If the iron content is unknown, it shall use the method 1 for accurate measurement. 5.3.6 Iron standard solution
5.3.6.1 Iron standard stock solution (0.500 mg/mL)
Weigh 0.500 g of metallic iron [wFe ??? 99.9%], into a 300 mL beaker (accurate to 0.0001 g). Add 30 mL of hydrochloric acid (5.3.1). Heat to dissolve it. Add 5 mL of nitric acid (5.3.2), to oxidize the iron. Continue to heat to drive off nitrogen oxides. Cool it down. Transfer it into a 1000 mL volumetric flask. Use water to dilute it to the mark. Mix well. 5.3.6.2 Iron standard solution (0.050 mg/mL)
Pipette 10.00 mL of iron standard stock solution (5.3.6.1) into a 100 mL volumetric flask. Use water to dilute it to the mark. Mix well. Prepare it when using. 5.4 Instruments
5.4.1 Analytical balance: Accurate to 0.1 mg.
5.4.2 Flame atomic absorption spectrometer: It uses air/acetylene flame; the wavelength is 248.3 nm.
5.5 Specimen
5.5.1 Specimen requirements
Sampling of sponge titanium, titanium, titanium alloys shall be carried out, in accordance with published standard methods.
5.5.2 Sample
Weigh 0.50 g of sample, accurate to 0.0001 g.
5.6 Analytical procedures
WARNING: Air-acetylene burners shall be ignited and extinguished, in
accordance with atomic absorption spectrometry instrumentation procedures, to avoid a possible explosion hazard.
5.6.1 Number of measurements
Two samples are measured independently. Take the average value.
5.6.2 Blank test
Carry out the blank test, by the use of pure titanium (5.3.5), along with the sample. 5.6.3 Preparation of standard solutions
5.6.3.1 General
The preparation of standard solution is carried out, according to 5.6.3.2 and 5.6.3.3. 5.6.3.2 wFe ??? 0.1%
5.6.3.2.1 Weigh 6 parts of pure titanium (5.3.5), 0.50 g per each part. Place them in a 200 mL polyethylene beaker.
5.6.3.2.2 Add 10 mL of hydrochloric acid (5.3.1) and 5 mL of hydrofluoric acid (5.3.3). Cover a polyethylene watch glass. Heat in a water bath to dissolve it. Add 3 mL of nitric acid (5.3.2). Heat to drive off nitrogen oxides. Add 3 g of boric acid (5.3.4). Stir to dissolve it. Cool it to room temperature.
5.6.3.2.3 Transfer the solution into a 100 mL volumetric flask. Add 0.00 mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00 mL, 10.00 mL of iron standard solution (5.3.6.2), respectively. Use water to dilute it to the mark. Mix well.
5.6.3.3 wFe > 0.1%
5.6.3.3.1 Weigh 6 parts of pure titanium (5.3.5), 0.50 g per each part. Place them in a 200 mL polyethylene beaker.
5.6.3.3.2 Add 10 mL of hydrochloric acid (5.3.1) and 5 mL of hydrofluoric acid (5.3.3). Cover a polyethylene watch glass. Heat in a water bath to dissolve it. Add 3 mL of nitric acid (5.3.2). Continue to heat to drive off nitrogen oxides. Add 3 g of boric acid (5.3.4). Stir to dissolve it. Cool it to room temperature.
5.6.3.3.3 Transfer the solution into a 100 mL volumetric flask.
5.6.3.3.4 Pipette part of the solution, according to Table 2, into six 100 mL volumetric flasks. Add hydrochloric acid (5.3.1). Add 0.00 mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00 mL, 10.00 mL of iron standard solution (5.3.6.2), respectively. Use water to dilute it to the mark. Mix well.
5.6.4 Preparation of test solution
5.6.4.1 Transfer the sample (5.5) into a 200 mL polyethylene beaker.
5.6.4.2 Add 10 mL of hydrochloric acid (5.3.1) and 5 mL of hydrofluoric acid (5.3.3). Cover a polyethylene watch glass. Heat in a water bath to dissolve it. Add 3 mL of nitric acid (5.3.2). Heat to drive off nitrogen oxides. Add 3 g of boric acid (5.3.4). Stir to dissolve it. After cooling, transfer the solution into a 100 mL volumetric flask. Use mL of water. Cool it.
6.3.7 Pure titanium: wTi ??? 99.95%: The iron content is known AND shall be as low as possible. If the iron content is unknown, it shall use the method 1, for accurate measurement.
6.3.8 Cobalt solution (1 mg/mL): Accurately weigh 1.00 g of pure cobalt (wCo ??? 99.5%), into a 300 mL beaker. Add 40 mL of nitric acid (6.3.3). Heat to dissolve it. Cool and transfer it to a 1000 mL volumetric flask. Use water to dilute it to the mark. Mix well. 6.3.9 Yttrium solution (1 mg/mL): Accurately weigh 1.27 g of yttrium trioxide (wY2O3 ??? 99.5%), into a 300 mL beaker. Add 20 mL of hydrochloric acid (6.3.1). Heat to dissolve it. Cool and transfer it into a 1000 mL volumetric flask. Use water to dilute it to the mark. Mix well.
6.3.10 Lanthanum solution (1 mg/mL): Accurately weigh 1.17 g of lanthanum trioxide (wLa2O3 ??? 99.5%), into a 300 mL beaker. Add 20 mL of hydrochloric acid (6.3.1). Heat to dissolve it. Cool and transfer it into a 1000 mL volumetric flask. Use water to dilute it to the mark. Mix well.
6.3.11 Iron standard solution (1.000 mg/mL): Accurately weigh 1.0000 g of metallic iron (wFe ??? 99.9%), into a 500 mL beaker. Add 60 mL of hydrochloric acid (6.3.1). Heat to dissolve it. Then add 10 mL of nitric acid (6.3.3), to oxidize iron from low valence to high valence. Heat it until no brown nitrogen and oxygen fumes are produced. Cool and transfer it into a 1000 mL volumetric flask. Use water to dilute it to the mark. Mix well.
6.4 Instruments
6.4.1 Polyethylene beakers and watch glass.
6.4.2 Polytetrafluoroethylene (PTFE) beakers and watch glass.
6.4.3 Analytical balance: Accurate to 0.1 mg.
6.4.4 Inductively coupled plasma atomic emission spectrometer: It shall have the ability to simultaneously measure Fe 238.20 nm, 259.94 nm, internal standard elements Co 228.62 nm, Y 371.03 nm, La 398.85 nm, Ti 255.60 nm or Ti 333.21 nm and other spectral lines. Hydrofluoric acid-resistant nebulizers are recommended, when nitric and hydrofluoric acids are used to dissolve the sample (6.6.3.2).
6.5 Specimen
6.5.1 Sampling
Sampling of sponge titanium, titanium, titanium alloys shall be carried out, in accordance with published standard methods.
6.5.2 Sample
Weigh 0.500 g of sample, accurate to 0.0001 g.
6.6 Analytical procedures
6.6.1 Number of measurements
Two measurements are performed independently. Take the average value.
6.6.2 Blank test
Carry out the blank test by the use of pure titanium (6.3.7), along with the sample. 6.6.3 Preparation of standard solutions
6.6.3.1 General
The preparation of standard solutions is carried out, in accordance with 6.6.3.2, 6.6.3.3 or 6.6.3.4.
6.6.3.2 Dissolution of specimens by nitric acid and hydrofluoric acid (applicable to 6.6.4.2).
6.6.3.2.1 Weigh 4 parts of pure titanium (6.3.7), 0.50 g per each part. Transfer them into a 200 mL polyethylene beaker.
6.6.3.2.2 Add 50 mL of nitric acid (6.3.3) and 10 mL of hydrofluoric acid (6.3.4). Cover a polyethylene watch glass. Heat it in a water bath to dissolve it completely. Continue to heat and boil it, to drive off nitrogen oxides. Cool to room temperature. 6.6.3.2.3 Remove the watch glass. Pipette 0.00 mL, 5.00 mL, 10.00 mL, 15.00 mL of iron standard solution (6.3.11), respectively. Transfer the solution into a 100 mL volumetric flask.
6.6.3.2.4 Add 5.0 mL of cobalt internal standard solution (6.3.8). Use water to dilute it to the mark. Mix well. Immediately transfer the solution into a dry polyethylene or polytetrafluoroethylene bottle, for preservation.
6.6.3.3 Dissolution of specimens by sulfuric acid and hydrofluoric acid (applicable to 6.6.4.3).
6.6.3.3.1 Weigh 4 parts of pure titanium (6.3.7), 0.50 g per each part. Place them in a 200 mL polytetrafluoroethylene beaker.
6.6.3.3.2 Add 20 mL of sulfuric acid (6.3.5) and 4 mL of hydrofluoric acid (6.3.4). Cover a polytetrafluoroethylene watch glass. Heat at low temperature to dissolve it. If the dissolution is not complete, it may add a small amount of hydrofluoric acid (6.3.4); continue heating at low temperature, until complete dissolution. Add 4 mL of nitric acid Continue heating to drive off nitrogen oxides. Cool to room temperature. 6.6.4.2.3 Remove the watch glass. Transfer the solution into a 100 mL volumetric flask. 6.6.4.2.4 Add 5.0 mL of cobalt internal standard solution (6.3.8). Use water to dilute it to the mark. Mix well. Immediately transfer it into a dry polyethylene or polytetrafluoroethylene bottle, for preservation.
6.6.4.3 Dissolution of specimen by sulfuric acid and hydrofluoric acid. Note: This method is applicable to the measurement of iron, in titanium (including commercial pure titanium) and titanium alloys.
6.6.4.3.1 Put the sample in a 200 mL polytetrafluoroethylene beaker.
6.6.4.3.2 Add 20 mL of sulfuric acid (6.3.5) and 4 mL of hydrofluoric acid (6.3.4). Cover a polytetrafluoroethylene watch glass. Decompose the specimen, by heating it at low temperature. If the dissolution is not complete, it may add a small amount of hydrofluoric acid (6.3.4); continue heating until the decomposition is complete. Add 4 mL of nitric acid (6.3.3). Heat it for 2 min ~ 3 min.
6.6.4.3.3 Remove the watch glass. Continue to heat until white smoke is emitted, for about 3 min ~ 5 min. Cool to room temperature. Use a small amount of water, to rinse the wall of the cup. Heat until it emits thick white smoke, for 2 min ~ 3 min. 6.6.4.3.4 The amount of sulfuric acid remaining in the beaker will affect the emission intensity. Therefore, it is recommended that the residual sulfuric acid volume shall be kept constant. The internal standard method can also be used, to eliminate the influence. 6.6.4.3.5 Cool to room temperature. Add 20 mL of hydrochloric acid (6.3.1) and a small amount of water, to dissolve the salts.
6.6.4.3.6 After cooling to room temperature, transfer it into a 100 mL volumetric flask. 6.6.4.3.7 Add 5.0 mL of cobalt (6.3.8), yttrium (6.3.9) or lanthanum (6.3.10) internal standard solution. Use water to dilute it to the mark. Mix well.
6.6.4.4 Dissolution of specimen by sulfuric acid (using titanium as the internal standard). Note: This method uses titanium as the internal standard; it is only applicable to the measurement of iron, in commercial pure titanium.
6.6.4.4.1 Put the sample in a 100 mL conical flask.
6.6.4.4.2 Add 40 mL of sulfuric acid (6.3.6). Slowly heat it, until the titanium is completely dissolved (add water to keep the volume constant). Add dropwise nitric acid (6.3.2), to oxidize titanium. Continue heating, until white smoke is emitted. Cool it to room temperature.
6.6.4.4.3 Transfer it into a 100 mL volumetric flask. Use water to dilute it to the mark. Mix well.
6.6.5 Measurement
6.6.5.1 General
6.6.5.1.1 Check the connection of each system. Turn on the instrument. Select the appropriate background correction position. Then ignite the plasma flame. Stabilize it for 30 min.
6.6.5.1.2 On the atomic emission spectrometer, use the internal standard method, to measure the emission intensity.
6.6.5.1.3 When the equipment has a computer system control function, THEN, the establishment of the working curve, calibration (drift correction, standardization, recalibration), measurement of iron content shall be carried out, in accordance with the requirements of the computer software operating instructions.
6.6.5.2 Drawing of working curve
The standard solution is measured by ICP atomic emission spectrometer. The emission intensities of iron and internal standard elements (Co, Y, La or Ti) are measured simultaneously, at the corresponding wavelengths, which are given in Table 3. According to formula (10), calculate the emission intensity ratio of iron and internal standard element.
Where:
R - The emission intensity ratio of iron and internal standard element; IFe - The emission intensity of iron;
IIS - The emission intensity of the internal standard element.
Use the mass concentration of iron (mg/100 mL) as the abscissa AND the emission intensity ratio as the ordinate, to draw the working curve. Make sure the linear correlation coefficient is better than 0.999. Move the relevant curve in parallel, so that it passes through the coordinate origin.

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