GB/T 6609.13-2026Chemical analysis and physical property determination methods for alumina - Part 13: Determination of calcium oxide content - Flame atomic absorption spectrometry (English PDF)

Foreword

This document complies with the provisions of GB/T 1.1-2020 "Standardization Work Guidelines Part

1.Structure and Drafting Rules of Standardization Documents". Drafting. This document is Part 13 of GB/T 6609, "Chemical Analysis Methods and Physical Property Determination Methods for Alumina". GB/T 6609 has been... The following sections were published.

1.Determination of Trace Element Content by Inductively Coupled Plasma Atomic Emission Spectrometry;

2.Determination of mass loss at 300°C and 1000°C;

---Determination of silica content by molybdenum blue spectrophotometry;

---Determination of ferric oxide content by o-phenanthroline spectrophotometry;

5.Determination of sodium oxide and potassium oxide content;

7.Determination of the content of titanium dioxide, chromium trioxide, copper oxide, fluorine, chlorine, boron trioxide, phosphorus pentoxide, and sulfate. Fixed-point spectrophotometry;

---Determination of vanadium pentoxide content by benzoylphenylhydroxylamine extraction spectrophotometry;

11.Determination of Manganese Monoxide and Magnesium Oxide Content by Flame Atomic Absorption Spectrometry;

12.Determination of Zinc Oxide Content by Flame Atomic Absorption Spectrometry;

13.Determination of Calcium Oxide Content by Flame Atomic Absorption Spectrometry;

19.Determination of Lithium Oxide Content by Flame Atomic Absorption Spectrometry;

---Determination of gallium trioxide content by butylrhodamine B spectrophotometry;

6 Instruments and Equipment

6.1 Flame atomic absorption spectrometer, equipped with a calcium hollow cathode lamp. Under optimal instrument operating conditions, flame atomic absorption spectrometers that can achieve the following specifications... Absorption spectrometers can all be used.

---Characteristic concentration. In a solution consistent with the matrix of the analytical solution, the characteristic concentration of calcium oxide is no greater than 0.5 µg/mL;

---Precision. The standard deviation of 10 absorbance measurements using the highest concentration standard solution should not exceed 1.5% of the average absorbance. The absorbance of the lowest concentration standard solution (not the "zero" concentration standard solution) measured 10 times should have a standard deviation not exceeding that of the highest concentration standard solution. 0.5% of the average absorbance of the standard solution;

---Linearity of the working curve. The working curve is divided into five equal segments according to concentration. The absorbance difference of the highest segment and the absorbance difference of the lowest segment are linear. The ratio is not less than 0.7.

6.2 Microwave digestion apparatus.

6.3 PTFE sealed sample container, schematic diagram shown in Figure 1.

6.4 The dryer uses activated alumina as a desiccant and should be activated at 300°C before each use.

6.5 Oven, temperature can be controlled at 300°C±10°C.

7 Samples

Sampling shall be carried out in accordance with the provisions of Chapter 6 of GB/T 6609.22-2026, and sample preparation shall be carried out in accordance with Section

7.4 of GB/T 6609.22-2026. The regulations shall be followed.

8 Test Procedure

8.1 Samples Weigh 0.25g of the sample (Chapter 7), accurate to 0.0001g.

8.2 Parallel Tests Perform two parallel experiments and take the average value.

8.3 Blank Test A blank test was performed along with the sample.

10 Precision

10.1 Repeatability Limit (r) The measured values of two independent test results obtained under repeatability conditions, within the range of the average values given in Table 1, represent the two test results. The absolute difference does not exceed the repeatability limit (r), and the number of cases exceeding the repeatability limit (r) does not exceed 5%. The repeatability limit (r) is determined by linearity of the data in Table 1. Obtained by interpolation or extrapolation.

11 Test Report The test report should include the following.

---Measurement content;

---Document number;

---Sample dissolution method;

---Analysis results and their representation;

---Differences from basic analytical procedures;

---Abnormal phenomena observed during the measurement;

13 Determination of Calcium Oxide Content Flame atomic absorption spectrometry

1.Scope This document describes a method for determining the calcium oxide content in alumina using flame atomic absorption spectrometry. This document applies to the determination of calcium oxide content in alumina. The determination range (mass fraction) is 0.0050% to 0.15%.

4.Method Overview The samples were dissolved using a PTFE-sealed dissolver or a microwave digester, in the presence of strontium or lanthanum salts as releasing agents. The absorbance of calcium oxide was measured at 422.7 nm using an air-acetylene flame atomic absorption spectrometer. The oxygen content was calculated based on the working curve. The content of calcium chloride.

5.Reagents Unless otherwise specified, only reagents confirmed to be of superior purity and Grade I water conforming to GB/T 6682 shall be used in the analysis.

5.1 Hydrochloric acid (1 1).

5.2 Sulfuric acid (1 2).

5.3 Strontium chloride solution (100 g/L). Weigh 100 g of strontium chloride monohydrate (SrCl2·H2O) and place it in a 250 mL beaker. Dissolve it in water. Transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix well. Store in a plastic bottle.