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GB/T 3286.1-2012: Methods for chemical analysis of limestone and dolomite - Part 1: The determination of calcium oxide and magnesium oxide content - The complexometric titration method and the flame atomic absorption spectrometric 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 3286.1: Historical versions
Similar standardsGB/T 3286.1-2012: Methods for chemical analysis of limestone and dolomite - Part 1: The determination of calcium oxide and magnesium oxide content - The complexometric titration method and the flame atomic absorption spectrometric 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/GBT3286.1-2012 NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 73.080 D 52 Replacing GB/T 3286.1-1998 Methods for chemical analysis of limestone and dolomite - Part 1.The determination of calcium oxide and magnesium oxide content - The complexometric titration method and the flame atomic absorption spectrometric method Issued on. NOVEMBER 05, 2012 Implemented on. MAY 01, 2013 Issued by. General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China; Standardization Administration of the People's Republic of China. Table of ContentsForeword... 3 1 Scope... 5 2 Normative references... 5 3 Complexometric titration method... 6 4 Flame atomic absorption spectrometric method... 18 5 Test report... 23 Annex A (normative) Flow chart of the acceptance procedure of sample analysis results... 24 Annex B (informative) Function relationships and raw data of precision test. 251 ScopeThis Part of GB/T 3286 specifies the determination of calcium oxide and magnesium oxide content by complexometric titration method and the determination of magnesium oxide content by atomic absorption spectrometric method. This Part applies to the determination of calcium oxide content and magnesium oxide content in limestone and dolomite. It also applies to the determination of calcium oxide content and magnesium oxide content in metallurgical lime. Complexometric titration method, determination range (mass fraction). calcium oxide content is greater than 20 %, magnesium oxide content is greater than 2.5 %; atomic absorption spectrometric method, determination range (mass fraction). magnesium oxide content is 0.1 % ~ 2.5 %.2 Normative referencesThe following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. GB/T 2007.2 General rules for the sampling and sample preparation of minerals in bulk - Sample preparation by manual method GB/T 3286.2 Methods for chemical analysis of limestone and dolomite - Part 2.The determination of silicon dioxide content - The silicomolybdic blue spectrophotometric method and the perchloric acid dehydration gravimetric method GB/T 3286.3 Methods for chemical analysis of limestone and dolomite - Part 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 7728 Chemical analysis of metallurgical products - General rule for flame atomic absorption spectrometric methods GB/T 8170 Rules of rounding off for numerical values & expression and judgement of limiting values3 Complexometric titration method3.1 Principle The sample is melted with sodium carbonate-boric acid mixed flux and leached with dilute hydrochloric acid. 3.3 Instruments Use common laboratory instruments and equipment. 3.4 Sample preparation 3.4.1 PREPARE samples according to GB/T 2007.2. 3.4.2 The samples shall be processed to a particle size of less than 0.125 mm. 3.4.3 Before analysis, limestone and dolomite samples are dried at 105 °C ~ 110 °C for 2 h, and then placed in a desiccator to cool to room temperature. 3.4.4 The preparation of metallurgical lime samples shall be carried out quickly. After the samples are made, they shall be immediately sealed in a ground- mouth bottle or plastic bag and stored in a desiccator. The samples are not be dried before analysis. 3.5 Analysis steps 3.6.2 Determination and representation of analysis results If the absolute value of the difference between the two independent analysis results of the same sample is not greater than the repeatability limit r value, the arithmetic mean is taken as the analysis result. 3.7 Precision The precision data is determined in 2011 by 8 laboratories on samples with 5 different levels of calcium oxide and magnesium oxide content. Each laboratory independently determines the calcium oxide and magnesium oxide content three times under repeatability conditions.4 Flame atomic absorption spectrometric method4.1 Principle The sample is decomposed with hydrochloric acid and hydrofluoric acid. Perchloric acid smokes and drives out the hydrofluoric acid. In the presence of strontium chloride, the test solution is sprayed into an air-acetylene flame. A magnesium hollow cathode lamp is used as the light source. The absorbance is measured at a wavelength of 285.2 nm of an atomic absorption spectrometer. 4.2 Reagents 4.2.1 Hydrochloric acid (1 + 1). 4.2.2 Hydrofluoric acid (ρ = 1.13 g/mL). 4.2.5 Magnesium oxide standard solution 4.3 Instruments Atomic absorption spectrometer, equipped with air-acetylene burner, magnesium hollow cathode lamp. The air and acetylene gas must be sufficiently pure (no water, oil, and magnesium) to provide a stable, clear flame. CHECK the performance of the atomic absorption spectrometer according to the requirements of GB/T 7728.The instruments used shall meet the following indicators. 4.3.1 Minimum precision requirements MEASURE the absorbance 10 times using the standard solution of the highest concentration, and calculate the average value and standard deviation of the absorbances. The standard deviation shall not exceed 1.0 % of the average absorbance. 4.3.2 Characteristic concentration The characteristic concentration of magnesium oxide shall be better than 0.007 μg/mL. 4.3.3 Detection limit The detection limit of magnesium oxide shall be better than 0.004 μg/mL. 4.3.4 Linearity of the calibration curve The calibration curve is divided into 5 sections according to the concentration. The ratio of the difference between the absorbance difference in the highest section and the difference in absorbance in the lowest section should not be less than 0.7. 4.4 Sample preparation 4.5 Analysis steps 4.5.1 Determination times For a same sample (4.4.3 or 4.4.4), determine at least 2 times independently. 4.5.2 Sample amount WEIGH 0.20 g of sample, to the nearest 0.0001 g. For metallurgical lime samples, the samples shall be quickly weighed. 4.5.3 Blank test CARRY OUT the blank test along with the sample. 4.5.4 Sample decomposition and preparation of test solution 4.5.4.3 Test solution 4.5.4.3.1 PIPETTE 10.00 mL of test solution (4.5.4.2) into a 100 mL volumetric flask, ADD 5 mL of hydrochloric acid (4.2.1) and 5.0 mL of strontium chloride solution (4.2.4), DILUTE to the mark with water, MIX well. This test solution is used for the determination of 0.1 % ~ 0.50 % of magnesium oxide content. 4.5.4.3.2 PIPETTE 20.00 mL of test solution (4.5.4.3.1) into a 100 mL volumetric flask, ADD 5 mL of hydrochloric acid (4.2.1) and 5.0 mL of strontium chloride solution (4.2.4), DILUTE to the mark with water, MIX well. This test solution is used for the determination of more than 0.50 % of magnesium oxide content. 4.5.6 Plotting of calibration curve PIPETTE 0 mL, 1.00 mL, 2.00 mL, 4.00 mL, 6.00 mL, 8.00 mL, 10.00 mL of magnesium oxide standard solution (4.2.5.2) respectively into a set of 100 mL volumetric flasks, each ADD 5 mL of hydrochloric acid (4.2.1) and 5.0 mL of strontium chloride solution (4.2.4), DILUTE to the mark with water, MIX well. At a wavelength of 285.2 nm of the atomic absorption spectrometer, ADJUST the zero point with water and measure the absorbance. PLOT the calibration curve with the concentration of magnesium oxide as the abscissa and the absorbance subtracting the zero-concentration solution as the ordinate. 4.6 Calculation and representation of analysis results 4.6.2 Determination and representation of analysis results If the absolute value of the difference between the two independent analysis results of the same sample is not greater than the repeatability limit r value, the arithmetic mean is taken as the analysis result. If the absolute value of the difference between the two independent analysis results is greater than the r value, increase the number of measurements and determine the analysis result as specified in Annex A. The analysis result is rounded off according to GB/T 8170, and the numerical value is rounded off to two decimal places. 4.7 Precision The precision data is determined in 2011 by 8 laboratories on samples with 5 different levels of magnesium oxide contents. Each laboratory independently determines the magnesium oxide contents three times under repeatability conditions.5 Test reportThe test report shall include the following contents. ......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 3286.1-2012 be delivered?Answer: The full copy PDF of English version of GB/T 3286.1-2012 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 3286.1-2012_English with my colleagues?Answer: Yes. The purchased PDF of GB/T 3286.1-2012_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. 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