GB/T 4698.2-2011 PDF EnglishUS$280.00 · In stock · Download in 9 seconds
GB/T 4698.2-2011: Methods for chemical analysis of titanium sponge, titanium and titanium alloys -- Determination of iron content 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 4698.2: Historical versions
Similar standardsGB/T 4698.2-2011: Methods for chemical analysis of titanium sponge, titanium and titanium alloys -- Determination of iron content---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/GBT4698.2-2011 GB NATIONAL STANDARD OF THE PEOPLE’S 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 ContentsForeword... 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... 241 ScopeThis 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 referencesThe 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 General3.1 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 6682.4 Method 1 -- 1,10-phenanthroline spectrophotometry4.1 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 4.3.4 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 4.4 Instruments 4.4.1 Analytical balance. Accurate to 0.1 mg. 4.4.2 Spectrophotometer. 4.5 Specimens 4.6 Analytical procedures 4.6.1 Number of measurements Carry out two measurements, independently. Take the average value. 4.6.2 Blank test Do a blank test with the sample. 4.6.3 Drawing of working curve 4.6.3.3 After standing at room temperature for 20 min, pipette part of the solution into a 1 cm absorption dish. Use water as a reference, to measure the absorbance of the standard solution. Use the mass concentration of iron (mg/100 mL) as the abscissa AND the absorbance as the ordinate, to draw the working curve. Make sure that, the linear correlation coefficient is better than 0.999.Move the relevant curve in parallel, so that it passes through the coordinate origin. 4.6.4 Measurement 4.6.4.1 Place the sample (4.5.2) in a 200 mL polytetrafluoroethylene beaker. 4.7 Calculation of analysis results The iron content is calculated in terms of the mass fraction of iron, wFe; the value is expressed in %; it is calculated according to formula (1). 4.8 Precision The tolerance of this method is represented by formula (2), formula (3), formula (4). Repeatability limit.5 Method 2 -- Atomic absorption spectrometry5.1 Measurement range The measurement range of iron is 0.01% ~ 2.00% (mass fraction). 5.2 Principle The specimen is dissolved with hydrochloric acid and hydrofluoric acid. The nitric acid titanium oxide, iron and other elements are added. Then boric acid is added; the iron concentration in the test solution is measured, by atomic absorption spectrometer. 5.3 Reagents 5.3.1 Hydrochloric acid (1 + 1). Slowly add 500 mL of hydrochloric acid (ρ1.16 g/mL ~ 1.19 g/mL) to 500 mL of water. 5.3.2 Nitric acid (1 + 1). Slowly add 500 mL of nitric acid (ρ1.42 g/mL) to 500 mL of water. 5.3.3 Hydrofluoric acid (1 + 1). Slowly add 100 mL of hydrofluoric acid (ρ1.14 g/mL) to 100 mL of water. 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 5.4 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 5.6 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 5.6.3.3 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 5.6.5 Measurement 5.6.5.1 General The instrument shall be equipped with an iron hollow cathode lamp, which is recommended by the manufacturer. The wavelength shall be set at 248.3 nm. The measurement shall be carried out, by an air-acetylene lean flame. When the equipment has a computer system control function, THEN, the establishment of the working curve, the calibration (drift correction, standardization, recalibration), the measurement of iron content shall be carried out, in accordance with the requirements of the computer software's operating instructions. 5.7 Calculation of analysis result 5.7.1 wFe ≤ 0.1% The iron content is calculated in terms of the mass fraction of iron wFe; the value is expressed in %; it is calculated according to formula (5). 5.8 Precision The tolerance of this method is represented by formula (7), formula (8), formula (9). Reproducibility limit.6 Method 3 -- Inductively coupled plasma atomic emission spectrometry6.1 Measuring range The measurement range of iron is 0.01% ~ 3.0% (mass fraction). 6.2 Method principles The sample is dissolved by nitric acid and hydrofluoric acid or sulfuric acid and hydrofluoric acid. The content of iron in the sample is measured, by inductively coupled plasma (ICP)-atomic emission spectrometer. 6.3 Reagents 6.3.1 Hydrochloric acid (1 + 1). Slowly add 500 mL of hydrochloric acid (ρ1.16 g/mL ~ 1.19 g/mL), into 500 mL of water. 6.3.2 Nitric acid (ρ1.42 g/mL). 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 6.5 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 6.6.4.2). 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. 6.6.3.3.6 Add 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. 6.6.3.3.7 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. 6.6.3.4 Dissolution of specimen by sulfuric acid (applicable to 6.6.4.4). 6.6.3.4.1 Weigh 4 parts of pure titanium (6.3.7), 0.50 g per each part. Place them in a 100 mL conical flask. 6.6.3.4.2 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 nitric acid (6.3.2) dropwise, to oxidize titanium. Continue heating, until the solution emits white smoke. Cool to room temperature. 6.6.3.4.3 Remove the watch glass. Add 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. Use water to dilute it to the mark. Mix well. 6.6.4 Preparation of test solution 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. 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. 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. ......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 4698.2-2011 be delivered?Answer: The full copy PDF of English version of GB/T 4698.2-2011 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 4698.2-2011_English with my colleagues?Answer: Yes. The purchased PDF of GB/T 4698.2-2011_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 4698.2-2011 -- 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 4698.2-2011?Answer: Yes. Unless special scenarios such as technical constraints or academic study, you should always prioritize to purchase the latest version GB/T 4698.2-2011 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 4698.2-2011?A step-by-step guide to download PDF of GB/T 4698.2-2011_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 4698.2-2011". 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 |
