This standard specifies the method for determining the amount of potassium oxide and sodium oxide by flame atomic absorption spectrometry. This standard is applicable to the determination of potassium oxide and sodium oxide in magnesium and magnesium-aluminum (aluminum-magnesium) refractory raw materials and products. The determination range is: the mass fraction of potassium oxide is 0.010% to 2.00%, and the mass fraction of sodium oxide is 0.010 to 1.00%. GB/T 5069.13-2001 Chemical analysis method for magnesium and magnesium-aluminum (aluminum-magnesium) refractory materials Determination of potassium oxide and sodium oxide by flame atomic absorption spectrometry GB/T5069.13-2001 Standard download decompression password: www.bzxz.net

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National Standard of the People's Republic of China
GB/T 5069..5069.13---2001
Chemical analysis of nagnesiu and magnesia-alumina refrattory materials
Chemical analysis of nagnesiu and magnesia-alumina refrattory materials20011217 Issued
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China
20020501 Implementation
GB/T5069.13—2007
This standard is modified for the determination of potassium oxide and sodium oxide content by absorption spectrophotometry for H/5.1035 steel.
This revision changes the chemical analysis method for magnesium refractory materials to the chemical analysis method for magnesium and lithium refractory materials.
This revision adds the chapters "Preface" and "Scope" and "Use of Standards" and adds the allowable error of standard samples in "Allowable Difference". The contents of this revision are as follows:
The determination range of the mass fraction of potassium monoxide and sodium monoxide is increased from 1% to 6.50% to 0.5% of the cumulative mass fraction of sodium monoxide, and the mass fraction of oxide is 9.10-1.0% without changing the determination conditions. Under the previous conditions, only the test volume is changed to expand the scope of determination. (t) The test solution is transferred to 5) 1ml, and the volumetric constant is changed to 100r:l. Volumetric flask constant. (2) (0) 0.20% (Na) C. 1 hour, take 10.0ml of the test solution and put it into 50ml of the volumetric flask.
In order to ensure the working time of the method, in order to list the selection of the method, this standard has 13 other sub-standards under the general title of chemical analysis method of magnesium and magnesium (aluminum magnesium secondary fire material): the main is the determination of the amount of
the determination of the dioxygen form by blue light Quantity:
Quantity of silicon dioxide by photometric method; Quantity of fluoride by o-dimethoxycarbonylation; Quantity of tin oxide by flame atomic absorption spectrophotometry; Quantity of aluminum oxide by EDTA spectrophotometry; Quantity of titanium dioxide by diaminobenzene spectrophotometry; Quantity of titanium dioxide by hydrogen peroxide spectrophotometry; Quantity of cobalt oxide by chromatograph; Quantity of calcium oxide by chromatograph; Quantity of zirconium oxide by flame atomic absorption spectrophotometry; Quantity of potassium oxide by flame atomic absorption spectrophotometry; This standard shall be replaced by GB569.11-1285 from the date of implementation. This standard is proposed by the National Refractory Bureau. This standard is jointly established by the National Technical Committee for Standardization of Refractory Materials. The drafting unit of this standard is: Luyang Refractory Research Institute. The main drafters of this standard are: Yao Wenmeng, Chang Qiuhong and Gu Qiban. This standard was first issued in April 2011.
National Standard of the People's Republic of China
Chemical analysis method for magnesium and magnesium-aluminum (aluminum-magnesium) refractories. Determination of potassium oxide and sodium oxide by flame atomic absorption spectrometry Union of magnesium and magnesium aluminum refraction inulerile materials Flnne uomic acid or sulfide spectrometry for determinintion of pulsating uxidanil nitrile enmlent: Scope
This standard specifies the range of residual oxidation amount, sodium oxide method GBT5069.13-2C01
This standard is applicable to magnesium pressure, and provides the determination of oxide layer and sodium oxide in magnesium materials and products. The mass fraction of the oxidized part is 0.10%~2.00%, and the mass fraction of the oxidized part is 3.010-1.n0%. 2. Reference standards
The following standards contain additional texts that constitute standard texts through reference in this standard. The versions shown at the time of publication of this standard are valid: The standard department that has adopted this standard shall discuss the possibility of replacing the following standards with new versions: GT/T2007-TR7 Sampling and preparation of mineral products B/15039.1-2 Chemical analysis method of magnesium and aluminum refractory materials GB/317187 General rules for atomic absorption spectroscopy GB/710.12-2001 Forming time of fire 3. Methods and specifications
After the sample is decomposed at the phase point of the commercial atmosphere, a correct solution is prepared. The absorbance at the wavelength of 7.5 and 53.0 nm is measured respectively.
4.1 Commercial acid 1 is prepared with high-grade pure sodium hydroxide.
4.2 Hydrogen hydride 1 g/ml: high-grade pure 4.3 High-grade acid 1.58 g/mL: high-grade pure
4. Potassium hydroxide (containing kg) Take 0.55% potassium hydride preheated at 4 ~ 1.51.99%, place it in a 5.0% water bath, transfer it to a 0.5% volumetric container, dilute it with water to the scale, and evenly place it in a plastic bag. 4.5 Oxygen standard liquid 0.1g/m3
0.0 ... 69.13—2001
Weigh 10g of 199.99% sodium chloride, which has been calcined at 150°C-500°C for 1h and cooled to room temperature, place it in a 250°C well, add 5ml of water and pour it into a volumetric bottle. Mix the water until it is evenly distributed in a plastic bottle. 4.
Take some sodium oxide solution (standard solution) and place it in a plastic bottle with a water content scale and shake it with a spoon.
4.8 Oxidation evaluation - sodium-3-nitrogen standard solution (pure KU10. Na05/mL) Transfer 4-200 sodium-3-nitrogen standard solution (4.7) into a container with water and transfer until the mixture is ready for use:
5 Apparatus
Atomic absorption spectroscopy: Air and sodium-3-nitrogen fast burner (pure enough to burn with potassium, sodium, hollow pole lamp) are available. The air and fast gas are pure (containing potassium, sodium, etc.) to provide a stable combustion method. The atomic absorption spectrum used should meet the following indicators. 5.1 Precision requirements
Take the highest possible absorbance of the standard non-sensitive material 10 times and calculate the average value of the photometric value and the standard band deviation. This standard should not be The average absorbance should be 5%. The standard solution should not exceed the average absorbance of the highest irradiation solution by more than 5%. 5.2 The standard deviation should be divided into five parts according to the increase of the highest absorbance difference and the lowest absorbance difference. The difference is smaller than 7.6. Sample preparation: E.1 Test sample is heated to a particle size of less than .mm according to 6110335/007. 6.2 The sample is dried at 135℃~110℃ for 2h and then cooled in a dryer at a low temperature. 7 Analysis steps 7.1 Determination of data Quantity
Two samples should be taken for analysis: 7.2 Test material
Take C. Sample [KO).2(N,015, then weigh the sample to the nearest .00n1, 7.3 Vacuum test
Follow the blank test.
7.4 Test reduction
All samples of the same type are separated and sent to the labeled quality control.
7.5 Fluidization
7.5.1. Place the sample on a platinum plate and use a small amount of water. Add 1ml of hydrogen 1.2), 2.3m. (1.:) Heat and decompose until the chlorine gas is high. Remove the cold water and add 2.0 (1.3) pure hot water. Remove the chloral and cool:
7 .5.2 Add 4-ml. acid 1.1), mL water, low temperature heating rate, remove and cool. 5.3 Transfer the concentrated formula to 1U. Benlixin, dilute with water to the scale, control to about. Say. Note (K) 02N.0 transfer 1.0ul test (.5 in 1 3ml according to the text, 1): use water to lightly expand, control, GB/T5069.13--2001
7.5.4 The atomic absorption spectrometer returns to K7iri.5 and 8S.0um, using the research gas-2 standard fire tube, according to SB/T7728, the instrument needs to be fully charged to the maximum state, and the results are tested by the curve method, using zero, respectively, and the empty test case and the test solution (7.5.3. The strong light strain is measured by high precision measurement method. The high calibration solution absorbance is measured by high precision measurement method. According to the provisions of 7.2 of GL/77281557, the two calibration solutions are measured by the high precision measurement method and the sample is analyzed by the analytical method.
7.5 The preparation of the weighted curve
Take 0.2.00mL, 4.CCmL, 8.00mL, 12.00mL, 16.00mL, 20.0The concentration is expressed in /ml. The concentration of potassium hydroxide (sodium oxide) obtained by the calibration curve is expressed in /m1. The identity of the test solution is expressed in units of:
The amount of sample is expressed in g.
8.2 High-precision measurement method According to formula (2), the mass fraction (K) or w(Na(%)
or:
(A - A
The concentration of potassium oxide (sodium hydroxide) in low-pressure standard solution, unit is /mT. The concentration of potassium (sodium) chloride in high-pressure standard solution, unit is /I. The absorbance of potassium oxide (sodium) in low-pressure standard solution
The absorbance of potassium (sodium) chloride in high-pressure standard solution is 1--or the absorbance of the wave;
V--the volume being tested, unit is mLF
The sample salt is taken, unit is nominal
8.3 Acceptance of analytical value
According to GB/T506 9.1-2 ((1) The provisions of 7.2 shall apply. 8.4 The arithmetic mean of the test rod efficiency analysis values ​​shall be the final result. WX
X100.......(2)
The result shall be rounded to two decimal places in accordance with the provisions of GB/T81?. The result lower than C.19% shall be rounded to three decimal places. 9 The difference between the test results of
shall not exceed 10 in Table 1 and Table 2, and the difference between the test results of
>0. 55~n. n
0. 1e~ n. 5n
Specifications of standard sample
Permissible value of sample
. 21
> 0. 50 --1. 30
>1. 65-- 2. 00wwW.bzxz.Net
>0. 05G~-0. 10
2-0.1C~.0, 50
>0. 5C--1. 00
GB/T 5069. 13 -7001
End of table)
Permissible value of standard sample
Electrode filling type
±3 915
Permissible mixing system of sample
Permissible basis of sample
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