This standard is applicable to the determination of copper content in ferromolybdenum. Determination range: 50.00～75.00%. This standard refers to the international standard ISO 4173-1980 "Steel-Determination of molybdenum content-Gravimetric method". This standard complies with GB 1467-78 "General principles and general provisions for chemical analysis methods of metallurgical products". GB 5059.1-1985 Chemical analysis method for ferromolybdenum Determination of molybdenum content by 8-hydroxyquinoline gravimetric method GB5059.1-1985 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Methods for chemical analysis of ferromolybdenumThe 8-hydroxyquinoline gravimetric methodfor the determination of molybdenumThis standard is applicable to the determination of iron content. Determination range: 50.00～75.00%. UDC 669.15'28
: 543.21 :546
GB 5059.1--85
This standard refers to and adopts the international standard ISO4173-1980 "Ferromolybdenum-Determination of content-Gravimetric method". This standard complies with GB1467-78 "General principles and general provisions of chemical analysis methods for metallurgical products". 1'Method Summary
Dissolve the weighed sample, separate the iron with sodium hydroxide, precipitate platinum in the form of hydroxyquinoline salt in the presence of EDTA and ammonium oxalate, filter, dry and weigh the aqueous hydroxyquinoline salt (MoO2 (C.HgNO)2]. 2 Reagents
Ammonium oxalate.
Hydrofluoric acid (specific gravity 1.14).
Nitric acid (specific gravity 1.42).
2.4Nitric acid (1+3).
2.5Hydrochloric acid (specific gravity 1.19).
2.6Hydrochloric acid (1+1).
Sulfuric acid (1+1).
2.8Ammonium hydroxide (1+1).
2.9Sodium hydroxide solution (46-48%): Prepare in a polyethylene beaker. Prepare and store in polyethylene bottles. 2.10 EDTA solution (10%): Weigh 10g of sodium ethylaminetetraacetate (CnHi.ON,Na·2H,O), dissolve it in water, dilute to 1000ml, and mix well.
2.11 8-Hydroxyquinoline solution (3%): Weigh 3g of 8-hydroxyquinoline, dissolve it in 12ml of glacial acetic acid, add 60ml of water and heat to about 40℃, add ammonium hydroxide (2.8) dropwise until a small amount of permanent precipitate is formed, then add glacial acetic acid dropwise to dissolve the precipitate, cool to room temperature, dilute to 100ml with water, and mix well. 3 Instruments
General laboratory instruments.
4 Sample
The sample should pass through a 0.125mm sieve.
5 Analysis steps
5.1 Tester
National Bureau of Standards 1985-04-15 Issued
1986-01-01 Implementationbzxz.net
Weigh the sample according to Table 1.
5.2 Empty self-test
Test with the sample.
GB5059.1-—85
Sample, 5
5.3 Determination
5.3.1 Place the sample (5.1) in a 150ml polytetrafluoroethylene (PTFE) beaker, add 10ml sulfuric acid (2.7), heat but not to boiling, add nitric acid (2.3) until the sample is dissolved and 0.5ml excess. Add 5ml hydrofluoric acid (2.2), heat and evaporate until sulfuric acid smokes for 15 minutes, cool , add 5ml hydrochloric acid (2.5) and 5ml nitric acid (2.3), heat for 10min and dilute to about 50ml. 5.3.2 In a 650-800ml tall beaker, add 50ml sodium hydroxide solution (2.9) and 50ml water. Heat to boiling, place a funnel with a neck length of 75mm and a neck diameter of about 1mm on the beaker, slowly pour the solution (5.3.2) into the beaker through the funnel and keep the sodium hydroxide solution boiling, rinse the PTFE beaker with 85-90℃ hot water, and the washing water is added to the solution through the funnel, rinse the funnel and the upper wall of the tall beaker, boil for 2-3min, dilute with water to about 450ml and cool, transfer the solution to a 500ml volumetric flask, dilute to the scale, and mix well. Dry the original tall beaker! Pour the solution in the volumetric flask into the original beaker and let it stand for 15-20min. Filter with fast filter paper (to remove the precipitate.
5.3.3 Take 100ml of solution (5.3.2), place it in a 400ml beaker, dilute to about 200ml, add 10ml EDTA solution (2.10) and 3g ammonium oxalate (2.1), slowly heat until the ammonium oxalate is dissolved, cool to room temperature, and adjust to pH 4.0 with hydrochloric acid (2.6) and ammonium hydroxide (2.8) (using a pH meter), and boil. Add 20ml 8-hydroxyquinoline solution (2.11), and ensure that the reagent is added. The solution continues to boil.
Note: It must be precipitated in a stagnant liquid. Otherwise, the precipitate is difficult to wash! The yield is high; if it is dried to a constant volume (even for 2 to 3 days), the recovery rate is sometimes lower.
5.3.4 Place it at 80 to 90℃ for 5 to 10 minutes with occasional stirring. Slowly filter it with a porous glass with a diameter of 5 to 10 μm. Use a glass rod with a rubber head to move all the precipitate on the wall of the beaker into the H vortex, and wash the precipitate in the crucible with about 100 ml of hot water at 80 to 90℃.
Note: When filtering, the speed of solution injection into the glass should be limited to the level of the solution in the glass. This is conducive to the washing of the glass and the absence of soluble salts in the precipitate.
5.3.5 Dry at 125℃ overnight, cool and weigh. Re-dry and weigh. Note: The precipitate after filtration should be washed with hot water or with a filter paper with a minimum of filtration time. 2 The dried precipitate or the precipitate with hydroxylamine should be placed in an effective desiccator before weighing and dried at room temperature. ③ Before using the glass, it should be washed several times with hot water, nitric acid (2.4) and finally water. Then at 125 (, the scale in the chamber after use is washed away with water, and a small beaker containing 5-10ml sulfuric acid (2.7) is placed, and the furnace is filled with nitric acid (2.3). The beaker is heated to remove sulfuric acid smoke, cooled and removed. Under slow filtration, about 10m of hot water is passed. Then press (and 2 places with the washed batch.
6 Calculation of analysis results
Press the calculated content of the components:
In the formula: m-
GB5059.1-85
(mj-m2）×0.2305
The mass of hydroxyquinoline molybdenum, g,
m2——The mass of the crucible, g,
mo-—The amount of sample, g;
-——The fraction ratio of the sample solution
0.2305-——The conversion factor of hydroxyquinoline copper to molybdenum. The analysis results are accurate to the second decimal place. The allowable difference
The difference in the analysis results between laboratories should not be greater than the allowable difference listed in Table 2. Table 2
50.00~60.00
60.00 ~75.00
Additional Notes;
This standard was proposed by the Ministry of Metallurgy of the People's Republic of China. This standard was drafted by Jilin Ferroalloys of the Ministry of Metallurgy. Allowable Difference
From the implementation of this standard, the original Ministry of Metallurgy Standard YB580-65 "Methods for Chemical Analysis of Ferrous Metals" will be invalid. 218
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