This standard specifies the method for determining the amount of manganese oxide by flame atomic absorption spectrometry. This standard is applicable to the determination of manganese oxide in magnesia and magnesia-alumina (aluminum-magnesium) refractory raw materials and products, with a determination range of 0.010% to 0.50%. GB/T 5069.12-2001 Chemical analysis method for magnesia and magnesia-alumina (aluminum-magnesium) refractory materials Determination of manganese oxide by flame atomic absorption spectrometry GB/T5069.12-2001 Standard download decompression password: www.bzxz.net

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National Standard of the People's Republic of China
GB/T5069.--5059.132001
Chemical analysis of magnesia and nagutsiaalumina refractnry malerials2001-12.17 Issued
Shandong People's Government
National Quality Supervision, Inspection and Quarantine Authority.
2002-05-01 Implementation
(B/1 5069.122001
This standard is based on GB/T6069.10--1585% wide range chemical analysis method for refractory materials atomic absorption spectrophotometry
This standard will be magnesium raw materials for chemical analysis of disaster villages as the preparation of state-owned iron and magnesium aluminum (lead magnesium> chemical analysis method for refractory materials
This standard is revised and added to the "front desk" and "energy" and "market standards" chapters, and "allowed tea A" has increased the standard sample allowed The present revision, while maintaining the working curve method, also lists the required adjustment methods for optional use: This revision includes 3 new methods for the chemical analysis of refractory materials (aluminum and iron) under the general heading of 1 year old method, including the re-plate method for the reduction of burning; the blue photometric method for the determination of carbon dioxide; the light emission method for the determination of silicon dioxide; the photometric method for the determination of iron oxides; the absorption spectroscopy method for the determination of iron ore in refractory materials: ruthenium azure S Spectrophotometric determination of calcium oxide; EDTA titration method for determination of titanium dioxide; atomic absorption spectrometry for determination of calcium oxide: dye titration for determination of calcium oxide; atomic absorption spectrometry for determination of sodium oxide and sodium monooxide. The standard shall be effective from the month of implementation. . 0--193. This standard is certified by the original National Refractory Industry Network. This standard is approved by the National Refractory Standardization Technical Committee. This standard was initiated by Luoyang Refractory Research Institute. The main authors of this standard are Wen Hui, Guo Qiuhong and Gu Qixu. This standard was first issued in January 19H5.
National Standard of the People's Republic of China
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This standard specifies the method for determining the amount of chemical in the form of pyrolysis atomic absorption spectrometry. GB/T5069.12--2U01
GD/TCO69.101H8
This standard is used for the determination of the amount of chemical in the total product of raw materials, such as pyrolysis materials and pyrolysis materials. The range is: %--0.0.Www.bzxZ.net
2Referenced standards
The texts contained in the following standards are cited in this standard and constitute the text of this standard. The version shown in this standard is valid at the time of use. All standards will be excluded. All parties using this standard should explore the possibility of using the latest version of the following standards. E/127-108 Colloidal minerals The collection and sample preparation of products is G1516.1-200 magnesium paste and transfer (armored iron) are purchased for fire-processed materials and the average burning reduction is determined by the chemical analysis method [BT7728-17 Metallurgical Product Chemical Analysis Fire Intensity Absorption Spectrum Standard G/18171987 Value is approximately based on GB/T10325-G1, the world's major product sampling inspection and testing standards 3. According to the requirements, the sample is decomposed with lactic acid-perchloric acid, and then the sodium hydroxide solution is used to make a solution: at the atomic absorption spectrum, the absorbance of the product is measured at 27srm. The sample is decomposed with hydrochloric acid-perchloric acid and the manganese oxide is directly determined. The silicon dioxide is preferably eliminated with a series of acids. 4 Reagents
4.1 Mixing agent: Take 2 parts of anhydrous sodium magnetic acid (optical grade pure) and 1 part of ground acid (super pure). Mix: 4.2 Hydrochloric acid (+1): Prepare with alternative grade hydrochloric acid. 4.3 Hydrogen acid (pH 1.15 g nl.): chemically pure
4.4 Hydrogen acid 1.68 g/l.2. First pure
45% pure hydrochloric acid solution: 2. Multi-view solution (4.1), 40 m.i. hydrochloric acid (4.2) was transferred to a 113:m1 volumetric flask, diluted with water, 4.6 Oxidizing agent (Mn 1.5 mg/mL) concentration 0.3872 metal button (called .995%), 23 m.i. 11% hydrochloric acid (4.2) was transferred to the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China on December 17, 2001, and verified on May 1, 2002
GR/T 5069.122001
Turn the bottle with water to the scale,
4.7 Manganese oxide standard solution (containing Mn/l.: transfer 20.00ml of standard oxidation solution (6) to 1000mL volume, dilute with water to waste, shake: gold thick calcium should be used before (1 some treatment, special surface oxide, 4 water wash, then use water, 3 change - 4 change: dry naturally for use, 5 instrument
atomic absorption spectrometer·equipped with air-fast burner, radiation change slow explosion. The gas produced should be pure enough, cold, suitable), moisture absorption The original absorption spectrum used for the purpose of providing accurate information should meet the following indicators: 5.1 The accuracy should be as low as possible. Measure the standard solution with the highest concentration 1 time and calculate the average value of its absorbance. The standard deviation should not exceed 1.5% of the half-mean value of the absorbance. Measure the standard solution with the lowest concentration, not the zero concentration standard solution, and calculate the standard deviation. The standard deviation should not exceed 0.5% of the half-mean value of the absorbance. 5.2 The calibration curve should be divided into equal parts. The highest version The absorbance difference is the ratio of the absorbance at the maximum value to the absorbance at the maximum value, not less than 0.6. Sample 6.1 Sample size is 6 nm. ? Place in a 1051~1U oven. Cool to room temperature. Analytical step 7.1 Determination of quantity 7.2 Take 1.1 sample (.1 mm) and weigh 0.001. 7.3 Test chamber test 7. 7.4 Test and analysis of the standard material. 7.5 Test and analysis 7.5.1 Wet the sample with water. Add 10% hydrogen peroxide (4.3) 2% high pressure (.4) heat to separate the gas under high pressure, cool, rinse with water, add 2% chlorine (4.4) to heat until the acid can be absorbed as much as possible. 7.5.7 Add 4% hydrochloric acid (small .2) and 1% water, heat to low temperature until the heat is dissolved, filter the sample with 7C6m volumetric flask, wash the mouth and swimming paper 3 times with hot water (this is the card liquid! .75.3 Place the mixture in a 18 jin (10 jin high temperature 10 10 000 mmol/l) solution and cool to 1.5.4. Add 6 ml of molten salt (4.2) in portions, with a little heat, take the molten material while heating, and pour the liquid into the main well 11.5.21, 2. Mixture-salt (1.5). Water dilution 15. GB/T5069.12—2001. 7.5.5 After 7.5.1 decomposition, add 8 ml of acid (1.2). 10 ml of water, heat until the salt is dissolved, remove, cool and pour into a 1 UVm container, and use a band to dilute to measure. 7.5 .6 At the atomic absorption wavelength of 273.5 nm, use the gas-type rapid adjustment, connect the instrument to GB/T7723, and after the instrument meets the performance requirements, if the test curve method is used, use water to zero, and test the absorbance of the sample box liquid (7.5.4 or ?..3), or if the high-precision measurement method is used, the standard calibration is reduced, and the test liquid (7.5.4 or 7.5.5), the light intensity of the calibration solution. Note: According to the conditions of (%2-87, the temperature of the same model should be multiplied by the value of the limit value of the element system and 5% lower than the value of the element system,
7.6 Calibration load drawing
f.6.1 Transfer 1.00ml..4.0umL.3.0)ml.7.30m1..9.03ml..123ml.3.20m1.35.30ml. Oxidation tank standard drop (1.) Place a group of 100mT. bottles, add 8aL (4.2, ml. mixture of hydrochloric acid and 14.3) and dilute with water to the scale, according to the sentence, according to 7.3. Measure its absorbance, draw the coordinate with the oxidation concentration less, and use the absorbance of the zero energy solution as the standard, and make the calibration line. 7.6.2# Take 0, 1.(0mL3.m.5.00al..7.0mL.KL-.L=3.mL15.00ml. Manganese dioxide standard solution (.7) and put them in 1.(1L dissolving bottle respectively, add 3ml salt solution (4.2) and dilute with water to the measuring point. Measure its absorbance according to 7.6, and convert the concentration of manganese dioxide into coordinates. The absorbance (minus the absorbance of the zero rise solution) is used as the coordinate to verify the calibration curve.
8 Expression of analysis results|| tt||8.1 Calibration method (1) Calculate the mass fraction of oxidized gas Mn-
Wherein, ——The rate of oxidation of the sample in the calibration curve is uP/mL. The unit of the calibration curve is /mV-The product of the concentration of the measured substance. The unit is ml.
The maximum test quantity should be:
82 High-precision measurement method (2) Calculate the mass fraction of oxidized gas e(M)
Wherein:
-(AA
The change of oxidation yield in the calibration fluid, the unit is ml. The change of oxidation yield in the calibration fluid, the unit is usually ml. The absorbance of the lower calibration fluid;
The absorbance of the higher calibration fluid:
The absorbance of the test solution!
The test report, the unit is I;
The maximum sample volume, the unit is.
8.3 Acceptance of analysis||tt ||Connect (D/T3059.12001, 7.2, 8.4, final result calculation and
sample effective analysis value of the drug is the technical average or final analysis result, V>10\-
fiber cool result connection CBT817\ rounded to one decimal place. The result is lower than 1.1, like about three digits of small dispersion, 9 allowable error
the difference of the analysis result is not significantly different from the original 1)
C. r50--c.15
20, 0 ~0.
20. 30-~0. 5c
:B,T 5069. 12—2001
standard
± 0. (007
二0. 03
test allowable error
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