GB/T 5195.1-2017 PDF EnglishUS$210.00 · In stock · Download in 9 seconds
GB/T 5195.1-2017: Fluorspar - Determination of calcium fluoride content - EDTA titration method and distillation-potentiometric titration method 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 5195.1: Historical versions
Similar standardsGB/T 5195.1-2017: Fluorspar - Determination of calcium fluoride content - EDTA titration method and distillation-potentiometric titration method---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/GBT5195.1-2017 GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 73.080 D 52 Replacing GB/T 5195.1-2006 Fluorspar - Determination of calcium fluoride content - EDTA titration method and distillation-potentiometric titration method Issued on. SEPTEMBER 07, 2017 Implemented on. JUNE 01, 2018 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 EDTA titration method... 6 4 Distillation-potentiometric titration method... 13 5 Test report... 18 Appendix A (Informative) Joint test raw data... 19 Appendix B (Normative) Flowchart of acceptance procedure of specimen analysis result... 20ForewordGB/T 5195 is divided into 16 parts. - Part 1.EDTA titration method and distillation-potentiometric titration method; - Part 2.Determination of carbonate content; - Part 3.Determination of loss in mass at 105 °C - Gravimetric method; - Part 4.Determination of sulfide content - Iodometric method; - Part 5.Determination of total sulfur content - The iodometric method after combustion; - Part 6.Determination of phosphorus content - Photometric method; - Part 7.Determination of zinc content - Flame atomic absorption spectrophotometric method; - Part 8.Determination of silicon dioxide content; - Part 9.Determination of loss on ignition - Gravimetric method; - Part 10.Determination of iron content - 1,10-phenanthroline spectrophotometric method; - Part 11.Determination of manganese content - The periodate spectrophotometric method; - Part 12.Determination of arsenic content - Atomic fluorescence spectrometry; - Part 13.Determination of aluminum content - EDTA titration method; - Part 14.Determination of magnesium content - Flame atomic absorption spectrometry; - Part 15.Determination of calcium, aluminum, silicon, phosphorus, sulfur, potassium, iron, barium and lead content - Wavelength dispersive X-ray fluorescence spectrometric method; - Part 16.Determination of silicon, aluminum, iron, potassium, magnesium and titanium content - Inductively coupled plasma atomic emission spectrometry. This part is Part 1 of GB/T 5195. This part was drafted in accordance with the rules given in GB/T 1.1-2009. This part replaces GB/T 5195.1-2006 "Fluorspar - Determination of calcium fluoride content". Compared with GB/T 5195.1-2006, the main technical changes of this part are as follows. - CHANGE the principle of the analysis method, from "When using EDTA standard titration solution for titration to the disappearance of green fluorescence, which is used as the end point; subtract the amount of calcium carbonate in the sample, to calculate the mass fraction of calcium fluoride in the sample" to "Take part of the filtrate under the condition of pH greater than 12.5, use EDTA standard titration solution to titrate calcium, to calculate the mass fraction of calcium fluoride” (see 3.1; 3.1 of the 2006 edition); - MAKE corresponding changes on the relevant reagents and analytical procedures (see 3.2 and 3.5; 3.2 and 3.4 of the 2006 edition); - CARRY out a common test of precision between laboratories, using the repeatability limit r and the reproducibility limit R obtained by statistics to replace the "allowable error" (see 3.6.2 and 4.6.2; 3.6 and 4.7 in the 2006 edition); - ADD the Appendix A "Raw data of common test" and Appendix B "Flowchart of acceptance procedure of specimen analysis results” (see Appendix A and Appendix B). This part was proposed by the China Iron and Steel Industry Association. This part shall be under the jurisdiction of the National Steel Standardization Technical Committee (SAC/TC 183). Drafting organizations of this part. Wuhan Iron and Steel (Group) Company, Metallurgical Industry Information Standards Institute. The main drafters of this part. Zhou Zheng, Wen Xiangdong, Chen Shihua, Zhang Suizhong, Wu Lixin, Yang Yan, Zhang Jinying, Wen Bin, Zheng Feng, Lu Chunsheng. This part replaces the standard previously issued as follows. - GB/T 5195.1-1985, GB/T 5195.1-2006. Fluorspar - Determination of calcium fluoride content - EDTA titration method and distillation-potentiometric titration method Warning - The personnel using this part shall have practical experience in formal laboratory work. This part does not point out all possible safety issues. The user is responsible for taking appropriate safety and health measures and ensuring compliance with the conditions stipulated by relevant national laws and regulations.1 ScopeThis part of GB/T 5195 specifies the methods for determining the content of calcium fluoride by EDTA titration and distillation-potentiometric titration. This part applies to the determination of calcium fluoride content in fluorite. EDTA titration method has a measuring range (mass fraction). ≥ 60%; distillation-potentiometric titration method has a measuring range (mass fraction). ≥ 90%.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) are applicable to this standard. GB/T 6379.1 Accuracy (trueness and precision) of measurement methods and results - Part 1.General principles and definitions GB/T 6379.2 Accuracy (trueness and precision) of measurement methods and results - Part 2.Basic method for the determination of repeatability and reproducibility of a standard measurement method GB/T 6682 Water for analytical laboratory use - Specification and test methods GB/T 8170 Rules of rounding off for numerical values & expression and judgement of limiting values3 EDTA titration method3.1 Principle The sample is leached with dilute acetic acid containing calcium, filtered, decomposed by one of the following two methods. 3.2 Reagents Unless otherwise specified in the analysis, only use approved analytical reagents and distilled water of grade 3 or higher that meets the requirements of GB/T 6682 or water of equivalent purity. 3.2.1 Sodium carbonate-boric acid mixed flux. take two parts of anhydrous sodium carbonate and one part of boric acid; grind and mix it uniformly. 3.2.2 Hydroxylamine hydrochloride. 3.2.3 Absolute ethanol. 3.2.8 Potassium hydroxide solution, 200 g/L. 3.2.9 Magnesium sulfate solution, 5 g/L. 3.2.10 Triethanolamine, 1 + 2. 3.2.11 Calcium fluoride standard solution, 0.0015601 g/mL. Weigh 1.0008 g of calcium carbonate ( > 99.99%) that has been pre-dried at 105 °C ~ 110 °C for 2 h and placed in a desiccator to cool to room temperature in a 250 mL beaker; cover a watch glass; slowly add 25 mL of hydrochloric acid (3.2.5). After the calcium carbonate is dissolved, add 100 mL of water; heat to boil it; drive off the carbon dioxide; cool to room temperature. Transfer the solution into a 500 mL volumetric flask; use water to dilute to the mark; mix it uniformly. 1.00 mL of this calcium standard solution is equivalent to 0.0015601 g calcium fluoride. 3.2.13 Mix the indicator, weigh 0.20 g of calcein (C30H26N2O13), 0.12 g of thymolphthalein (C28H30O4), and 20 g of anhydrous potassium sulfate in a mortar; grind them fine and evenly; transfer to a suitable container; place it at 105 °C ± 5 °C to dry it for 1 h and cool it down. Store in a mouth-ground bottle for later use. 3.4 Sample preparation 3.4.1 Prepare specimen according to GB/T 22564. 3.4.2 The specimen shall be processed to a particle size less than 0.063 mm, dried at a temperature of 105 °C ± 5 °C for 2 h, placed in a desiccator to cool to room temperature. 3.5 Analytical procedures 3.5.1 Number of determinations For the same specimen (3.4.2), make at least 2 independent determinations. 3.5.2 Sample amount Weigh 0.50 g of specimen, accurate to 0.0001 g. 3.5.3 Blank test Do a blank test with the sample. 3.5.4 Sample decomposition 3.5.4.1 Alkali fusion4 Distillation-potentiometric titration method4.1 Principle In the presence of perchloric acid, the fluorine in the sample is separated by distillation with water vapor at 135 °C ± 2 °C through a temperature control device; the distillate is absorbed by sodium hydroxide solution; the fluoride ion selective electrode is used as the indicator electrode; the lanthanum nitrate standard titration solution is used to titrate the amount of fluorine in the distillate, to calculates the mass fraction of calcium fluoride. 4.2 Reagents Unless otherwise specified in the analysis, only use approved analytical reagents and distilled water of grade 3 or higher that meets the requirements of GB/T 6682 or water of equivalent purity. 4.2.1 Potassium permanganate, crystalline. 4.2.3 Ethanol or isopropanol. 4.2.4 Perchloric acid, ρ = 1.67 g/mL. 4.2.5 Perchloric acid, 1 + 6. 4.2.6 Sodium hydroxide solution, 40 g/L, stored in a plastic bottle. 4.2.8 Buffer solution, pH 6.5. Dissolve 140 g of hexamethylenetetramine in about 800 mL of water; use perchloric acid (4.2.5) to neutralize to a pH of 6.5 ± 0.2; use water to dilute it to 1000 mL; if necessary, adjust the pH to 6.5. 4.2.9 Phenolphthalein solution, 5 g/L, prepared with 95% ethanol (volume fraction). 4.3 Device 4.3.1 General laboratory equipment and gas generation and absorption devices. 4.3.2 The distillation device consists of a steam generator, a distillation flask, a condenser tube, two electric heating jackets, a contact thermometer with a relay, as shown in Figure 1, which can control the temperature of the distillation flask to 135 °C ± 2 °C. 4.3.3 Magnetic stirrer. 4.3.4 pH meter, equipped with glass electrode and saturated calomel electrode. 4.3.5 Burette, 20 mL, graduation interval 0.02 mL. 4.3.6 Fluoride ion selective electrode. 4.3.7 Reference electrode, saturated calomel electrode or other types of electrodes. 4.5.5 Potentiometric titration Pipette 50.00 mL of test solution from a 500 mL volumetric flask in a 250 mL beaker; add 10 mL of buffer solution (4.2.8) and 60 mL of ethanol (or isopropanol) (4.2.3). Put the rotor of the magnetic stirrer into the beaker; place the beaker on the stirrer; insert the fluorine ion selection electrode (4.3.6) and the reference electrode (4.3.7); connect the potentiometer (4.3.8). Start the magnetic stirrer; use lanthanum nitrate standard titration solution (4.2.7) to titrate it; the titration speed is not more than 3.0 mL/min; record the volume of the titration and the corresponding potential reading. When the potential change speed increases, titrate at a slower speed. Determine the end point of the titration from the drawn or recorded titration curve. 4.6 Calculation and presentation of results 4.7 Precision The difference between two independent measurement results under repeatability conditions is not greater than the repeatability limit r specified in Table 2.5 Test reportThe test report shall include the following.Appendix A(Informative) Joint test raw data The precision data was determined in 2015 by 8 laboratories on 5 specimens of different levels of calcium fluoride in fluorite. Each laboratory measures the calcium fluoride content of each level independently three times under repeatable conditions.Appendix B(Normative) Flowchart of acceptance procedure of specimen analysis result The flowchart of acceptance procedure of specimen analysis result is as shown in Figure B.1. ......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 5195.1-2017 be delivered?Answer: The full copy PDF of English version of GB/T 5195.1-2017 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 5195.1-2017_English with my colleagues?Answer: Yes. The purchased PDF of GB/T 5195.1-2017_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 5195.1-2017 -- 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 5195.1-2017?Answer: Yes. Unless special scenarios such as technical constraints or academic study, you should always prioritize to purchase the latest version GB/T 5195.1-2017 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 5195.1-2017?A step-by-step guide to download PDF of GB/T 5195.1-2017_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 5195.1-2017". 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 |