GB/T 3286.3-1998 Chemical analysis methods for limestone and dolomite - Determination of alumina content
Some standard content:
GB, T3286.3—1998
This standard is attached to xx6.—, cloud chemical analysis method Y content in the responsibility measurement and exchange, 266.5-1992 limestone, A cloud petrochemical season classification legal person: do the time fee record> trace order. Car method fast order will see the level of individual international separation · individual model standard · etc. "Unique wisdom this, the first calculation of Shu Tiangu Guang degree, the need for the second need EA determination transmission. This you 1A full non-equivalent to 1150154 petrochemical division square sent to China F wine sales measurement treasure oxygen excess method,
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GD, 326, credit package refers to the following standards: GE, T3266.】System chemical single chemical quantity determination
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GUT 5226.3 frequency moment quantity within the deputy extension:
GR/3256.+chemical baking benefit formulation 1
GK/T 3286. 5
chemical property determination!
GB/T 3286.6
Determination of exact quantity:
Definition of profit!
GRT 32A6. H
Research and development of the determination of the world:
GRT J2s6. H
Determination of the amount of carbon dioxide
This international standard is self-contained and is available in GB/T286.;--1082G132366J982. This standard is issued by the People's Republic of China. The original source is the industrial column of the Northern China. The drafting unit is: Wuhan (China) Company Technology Center. The drafting person of this standard is also the performance, Fang Zhongke, Zhang Rong, and the inspection and inspection. The lathe bed is 12F.
1 Fanyuan
National Standard of the People's Republic of China
Chemical analysis method of limestone and natural stone
Determination of the amount of alumina
Methads for cheruical analyais This standard specifies the determination of aluminium oxide content by the S optical disc method and the ELITA elimination method. GB/T 3286.31998
C32x6.519
GN/T 39×6.6-192
This standard is applicable to the determination of aluminum oxide content in quartz and dolomite, and also applies to the determination of ammonium hydroxide in lime. The first is the chromatographic method, the determination range is: aluminum oxide content 0.010~0.% The second is the ionization method, the determination range is: lead oxide content greater than 0.50%:
2 Referenced standards
The texts contained in the following standards are the provisions that are referred to in this standard: When this standard is published, the versions shown are valid. All standard parts will be revised according to the circumstances, and the parties using this standard should use the latest versions of the following standards in accordance with the relevant provisions. GB/T2007.2-138 Sampling and sample preparation of bulk mineral products - Manual sample preparation method GB/3286.1-1998 Chemical analysis method of limestone and dolomite - Determination of the content of magnesium oxide and magnesia GB/T3286.2-1998 Chemical analysis method of limestone and dolomite - Determination of the content of silicon dioxide GB/T3286.4-1998 Chemical analysis method of limestone and dolomite - Determination of the content of lead monoxide - Part 1 - Spectrophotometric method
3 Summary of the method
The sample is melted with sodium carbonate-hydrogen peroxide as a baking agent, and the total amount is taken with hydrochloric acid. A portion is taken for testing, and potassium-hydrogen peroxide is used to carry out the removal of ions such as iron and manganese. In a six-stage ion exchange system, it reacts with sodium peroxide to form a purple-red complex, and the spectrophotometry is measured at a distance of 55 m from the spectrophotometer. The interference caused by the lack of lead can be eliminated by adding hydrogen peroxide solution. 4.1 Mixed flux, collect two ethylenediamine tetraacetic acid solutions and grind them wet, 4.2 Trichloroacetic acid (1+5): 4.3 Hydrochloric acid (+14): 4.4 EDTA: Take 2.76 potassium oxide in a 250ml beaker, add 100ml water, 6ml hydrochloric acid (1+1), heat, cool to room temperature, 5.5g disodium ethylenediaminetetraacetic acid in a 500: beaker, 2011ml water, add 1ml water (1+1), approved by the State Administration of Quality and Technical Supervision on December 7, 1998, and implemented on July 1, 1999. GB/T3286.31998. Heat and dissolve, cool to room temperature, mix the two liquids, add salt (1-1) and 11% water. 4.6 Add 5g of H2O2 to 10mL of static inventory, in order to find the coupling agent, check the package. 4.5 Filter hexamethylenetetramine (25%/1.), some in a plastic bottle. 4.6 Add 5g of oxidizing agent (5g) to a plastic bottle. 4.7 Dissolve hydrogen peroxide (3g), 4.B has S (1/L), prepare with ethyl acetate (1 +), and use it within one week after preparation. 4.9 Add 0.105% aluminum (not less than 90%) of tetrahydrofuran (5uml) to a cup, avoid heating, cool, add hydrochloric acid (1-1) to neutralize until it is clear, and then add 20ml of excess acid. Heat until the solution is clear, and cool. Add the solution to a 10ml container, Dilute with water, add 1.00200g of aluminum oxide. 4.5.2 Transfer 23.00ml of sodium hydroxide standard solution (4.9.) to a 16ml volumetric flask, add 10ml of hydrochloric acid (1/1). Dilute with water to a mark, add 1.09m of sodium hydroxide. 4.9.3 Transfer 19.00ml of sodium hydroxide standard solution (4.9.1) to a 10ml volumetric flask, add 1ml of hydrochloric acid (1+1), dilute with water to the mark, mix to make 2.0-5.0ml of aluminum oxide. 5 Instruments
During the analysis, no conventional laboratory air conditioner or equipment was used. 5 Sample preparation
According to GB/T2007.2, sample preparation
6.1 The sample should be processed until the particle size is less than u.125mm. 6.2 Before analysis, the samples of limestone and quartz should be dried at 1000 °C for 2 h, placed in a desiccator and cooled, and then filtered. 6.3 The preparation of samples of quartz should be carried out quickly. After preparation, the samples should be immediately sealed in ground-mouth bottles or plastic bottles and stored in a refrigerator. The samples should not be dried before analysis. 7.1 Weigh 0.5% sample on the test plate and accurately add 0.0% CO. For metallurgical limestone, the sample should be weighed quickly. 7.2 Blank test 7.3 Preparation of sample and stock solution 7.3.1 Mix the test solution (7.1) with 3.0 g of mixed molten platinum (4.1) and add 1.6 g of mixed baking agent (4.1). Place the platinum in a furnace with a temperature lower than 31°C, cover it with a platinum cover (leave it on), raise the furnace temperature to 959°C/1°C, melt for 10 min, heat the platinum, cool it, rinse it with water, and then place the block and the platinum mold in a 300ml beaker. Heat the melt at low temperature until the liquid is clear, cool it in a single chamber and transfer the mixture to a 20min cooler. Dissolve it in water until the solution is thick. This incubation is used as a stock solution for determining the amount of lead hydride, magnesium oxide, ferrous oxide and ferrous oxide. 4H328.1 Determine the amount of lead hydride and magnesium oxide by combining the two determinations. B/1256.3 Determine the amount of silicon dioxide by the uniform blue concentration method. h/13296. The product is determined by oxidation culture. CB, T3286.4 o-two mouse hybrid photometric cell to determine the chemical composition of the test peak currency, each of the new sugar preparation solution prepared by the state can be used for the test ring, the sample is divided into 7.4 determination method
.4.1 data into the sample containing lead, change the table 1 to take two portions of the reserve range <7.3.2) of 50m, the volume is full, one for color chain, one for replacement ratio reduction.
GB/T3286.3-1998
containing 0.25%~0.75 alumina, collect 20.0CmL reserve (7.8.2) in a =u1m. volume bottle, add 16mJ. hydrochloric acid 4. month water to the scale, mix. After the benefit, take two more portions 1.0m1, test filter in: 1000ml replacement bottle: constant aluminum content, system
0. 030. ~0. 030
20, ot-3. 2.
0, 25--n,75
20.36X<10/10(0)
hexamethylenetetramine solution, ml
blood self-dissolving R
7.4.2 color change, = zinc-) "A drop (4.4), mix, place for 3iu add 2.m). Grid big drop liquid (4.H) add hexamethylenetetramine gel (4., dilute with water to select scale, gently muddy about>0min, test the book in the presence of, in zinc-) TA wave (.4) add six drops of hydrogen peroxide solution (4.7). 7.4.3 more cut: time 2.1.2 Measure the absorbance of the color developing solution at 4°C using a spectrophotometer. Draw the corresponding curves on the working curve. According to the amount of aluminum oxide in the formula, take several blank test portions from Table 1 and select 100, 2.10, 2.03.4.00, 5.00mL of lead oxide standard solution (4.5.31 or 1.00.2.4.0), 5.00, 8.00mL respectively. mL oxidation period standard and drop solution (4.9.2). The following operations are the same as 7.1.2. Take another empty test drop according to? .4.3 Operation Prepare a weighed solution, select a sample with appropriate absorption, and measure the absorption rate at 545 aml of the spectrophotometer. With the amount of aluminum oxide as the horizontal coordinate and the absorption as the vertical coordinate, draw a curve. The average white fraction of the daily analysis results is calculated according to formula (1): a0,%) -
reserve volume +: L:
equivalent! Volume of reserve solution, m.: t.
Allowable difference
The amount of aluminum oxide obtained in the work, the test volume.
The difference between the independent analysis results in the laboratory and the difference between the actual analysis results should not be greater than the corresponding allowable difference listed in Table 2. For the new Jinshidong sample, no allowable difference between experiments is made. %
0. n~.0. n
2U. F0~~J. 75
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real treasure F volume
second routine
EDTA titration
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test play with two acid-acid mixture melt, acid method: with high-low-methylenediamine separation, iron or calcium precipitate and 52
CB/T3286:3-1998
calcium to obtain separation. Precipitate acid solution. Add excessive EIFA and other element ions, take monotonic as an indicator, use zinc standard to determine the excess ETA, and then use oxidized sodium to determine the ETA combined with aluminum: use standard dye to determine the excess. Titrate the anti-women, add benzoic acid to remove its influence, bZxz.net
11 Reagents
11.1 Mixing flux: Take 1 part of anhydrous carbonyl sodium]-1 part of static acid, grind again, mix 11.2 sodium argentate.
11.4 Salt bomb: 1+1).
51+2),
several water (93g7).
6 times distill tetramine solution (250ml) in 30% hygroscopic water. Add 11.T0 iron in this solution, take 0.35% nitrate powder in a 2s0nL beaker: add 2Jml. or (11.4) heating solution, add 1 drop of nitric acid (1.428/mL) to the solution: cool, pour the solution into a 5mL volumetric flask, dilute with water to a constant temperature. This solution contains 1.M trichlorfon solution (2g/mL).
11.12 ethyl acetate solution, add 3000ml of ammonium hydroxide, add 10g/mL of ethyl acetate, and dilute to 1. Use 11.4% ethyl acetate and 11.8% ethyl acetate to adjust the pH to 5.3-6.0: 1.13% sodium ethylenediamine (EETA)/EDTA (EDTA) = 1.14% methyl ether (1 P Ting.),
11.15 Diphenol according to the tower liquid (2 = 1) to the brown bottle: after the liquid is prepared, the time should not exceed 1 year - Shang: 1116 bell standard night / e (2n) -.093m01/7 you take 0.8189g850c explosion 2m and cool to Wangcheng high-purity zinc (not more than 999%) placed in a 5ml. beaker. A little water moistened 16mL European energy (.4) and heated to dissolve add 100mL water, add 2,4-diphenol (2 /.7. Preparation) and neutralize with water (11.7) until the liquid turns yellow. Use hydrochloric acid 1.5) and until it is colorless, and pass through 3~-6 full. Put the liquid into the grid! 00mm). Pass the bottle, dilute with water to the scale, and mark.
12 During the analysis, all experimental instruments and equipment were used. 73 Samples were prepared according to 5/72007.2. 13.1 The sample should be heated to a viscosity less than 0.1 nL/13.2 The sample for analysis was cooled to air in a neutralizer at 105~11°C for 2h. 13.3 The preparation of the sample should be carried out in reverse osmosis. After preparation, the sample was immediately placed in a flask or a sealed container and stored. The sample did not dry before separation.
14 Analysis steps
4.1 Material quantity: Take the sample according to the table according to the content of oxidizing agent in the sample and concentrate it to 0CC. For the test of the travel gold name spirit, the test material should be weighed quickly: 52
calculated weight
6.53~1.03
>1. --2. x
14.2 white test frequency
short test with the sample
14.3 test frequency
GB/T 3286. 3
Wu Ke Hai
Hold the amount of treatment·B
14.3.7 Put the sample (14.12) in platinum, add the melting point of Table 3, 11.1), homogenize, and then place in a high temperature furnace (11.1) with a temperature of less than 3 °C for a period of time, and gradually increase the melting point (intermittently) to 10 °C. Melt at this temperature for 13 min, take it out and turn it to dry, and cool it. 14.3.2 The homogenized platinum is placed in a 300 mL beaker, and 40 mL of hot acid (1=.1). Heat to remove the olefin block, and collect the platinum Equalizing cover: rinse with hot water. Heat to dissolve the block: boil the air test to remove light, cold part: when the amount of trimetallic iron in the sample is less than 3%, add 3ml of the test solution. Solution (11.10), 14.3.3 water to release the test plate to 150m, such as 1~2 methyl acceptors (1.14). Add 5L of hexamethylenetetramine (111.9) and use oxygenated water (11.7> to neutralize until the solution turns yellow, add chlorine (11.4) drop by drop until the solution turns red and add 3~4 excess. Stir continuously and add 2CL hexamethylenetetramine (11., heat to boil 1～2min, remove, cool, and after the precipitation has settled, use quick distilled water to avoid heat and then wash with hot oxidation (11,! 1) and discard the fever. --3 drink, 14.3.4 stick the paper on the original cup. Use hot water to precipitate and pour into the cup, old 30ml. Tropical acid (11.5) fractionally decompose the remaining precipitate: wash the filter paper with hot hydrochloric acid (11,6). Heat to completely decompose the precipitate, transfer the test solution into the 5-centimeter cone, and control the volume of the test solution to about 120mL.
14.3.5 Add D F4 drop roll (11.13) The amount should be based on the drop flow iron, the book will be higher than the complete combination and excess 3-5mL, standard sentence. If the fluorine contains n-1~ titanium dioxide, after adding FYTA drop liquid, add 16g of hydroxy acid (11.5), heat to dissolve. 14.3.6 Add 1 methyl orange drop liquid (-1.14), add or water, 11.7) to neutralize most of the acid, then add hydrogenated water (11.8) until it is fully dissolved and turns food color, add 10ml. wake-up-sleep fast-inhalation dissolution night (11.12), heat the surface for 2-~3min. Remove, run water and cool to room temperature. 4~5 drops of dimethoate solution (11.15) + use zinc standard solution (1.16) to titrate until the test sample changes from yellow to slightly red. If there is ethyl in the test sample, it will take time to titrate until the test sample turns slightly red. Add about 0.8 g of 143% ethanol for 11 minutes and add 5M 7-nitropropene to rinse the sample (11.12). Remove the sample 2-3 times, cool to room temperature, add 2-3 times of dialdehyde to dissolve the solution (11.15), and use standard solution (31.16) Titrate until the end point is equal to the red color of the excited part. Record the volume of the zinc standard drop consumed in the first titration, 15 Analysis of the results
Formula (2) Calculate the mass percentage of aluminum oxide: A,0, (%) = -F × G.050B
Where: V. The volume of the standard sample consumed by the titration, nIL: The volume of the blank solution to eliminate the zinc standard concentration, mI. The sensitivity of the zinc standard solution mo!/I.1
Test subject
J.098--with 1. needle standard box minus) 1./L equivalent to the quantified lead mass expressed in grams. 72
16 allowable full
GB/T3296.3-*998
The experimental determination within a practice point new random difference and two real full space analysis station stem value day should be people, Table 1 can list the allowable list, for metallurgical core also qualified, no experimental to the tolerance requirements, Table 4
Chemical inspection
n =a- -1. ck
There is no tolerance in this space
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