Some standard content:
Professional Standard of the People's Republic of China
ZBD51004—86
Adjusted to: 37-86
Analytical methods for serpemtine ores
Analytical methods for serpemtine ores :1986—12-20 Issued
Approved by the Ministry of Chemical Industry of the People's Republic of China and implemented on September 1, 1987
Professional Standard of the People's Republic of China
Analytical methods for serpentine ores
Analytical methods for serpentlne oresZBD51004-86
Adjusted to HGh35)5-1986
This standard applies to the determination of silicon, calcium, magnesium, aluminum, nickel, iron, adsorbed water content and ignition loss in serpentine bamboo ore. 1 Determination of silicon content in serpentine ore (perchloric acid dehydration weight method) This method is based on 1S05890-1981 "Determination of silicon content in manganese ore and concentrate - weight method" 1.1 Method summary
The sample is decomposed with hydrochloric acid, the residue is melted with sodium carbonate, leached with the original solution, and evaporated with perchloric acid. The silicate is dehydrated, quenched, burned, weighed, and silicon is removed by adding hydrofluoric acid. The content of silicon dioxide is calculated from the weight difference before and after the hydrofluoric acid treatment. 1.2 Reagents
1.2.1 Anhydrous sodium carbonate (GB 639-77) 1.2.2 Hydrochloric acid (GB 622-77): pl.198/ml (1 + 1) 1. 2.3 Hydrochloric acid (5 + 95) 3
1.2.4 Perchloric acid (GB623-77): 70%) 1.2.5 Sulfuric acid (GB 625-77): P1.84g/ml 1.2.6 Hydrofluoric acid (GB620-77), 40%. 1.8 Sample
The sample is passed through a 106mm sieve, dried at 105-110℃ to constant weight, and placed in a desiccator. 1.4 Analysis steps
1.4.1 Weigh 0.5g of the sample (accurate to 0.00028) and place it in a 25ml beaker. 1.4.2 Add a small amount of water to moisten the sample, cover the surface III, slowly add 30ml hydrochloric acid (1.2.2), place on the electric hot plate, heat to a slight boil, rinse the surface blood with a small amount of water, filter with medium-speed quantitative filter paper, and wash the beaker and residue with hot water 3 to 4 times each. Transfer the filtrate and washing liquid to the original beaker for storage.
1.4.3 Transfer the residue and filter paper to platinum, dry carefully, ash, place in a muffle furnace, burn at 850℃ for 30min, take out and cool.
1.4. Add 3g anhydrous sodium carbonate (1.2.1), mix well, cover with 1g anhydrous sodium carbonate, cover with a volute cover, place in a muffle furnace and melt at 950C for 30min. Take it out, cool it down, put the crucible into the original beaker and heat it at low temperature to extract it, wash it out with water and cover it, add 20ml perchloric acid (1.2.4)
1.4.5 Cover 1. (leave a gap), place it on the electric heating plate, heat it until thick white smoke of perchloric acid comes out for 15 minutes, take it down and cool it down (because the perchloric acid is used in large quantities, pay attention to ventilation and safety). 1.4.6 Add 5ml hydrochloric acid (1.2.2), 50ml hot water, rinse the surface III with a small amount of water, stir to dissolve the salt, filter it with medium-speed quantitative filter paper, wipe the precipitate on the wall of the beaker with a glass rod with an eraser head, merge it on the filter paper, wash the precipitate with hot hydrochloric acid (1.2.3) 5~6 times, and then wash it with warm water for more than 10 times, and keep the filtrate and washing liquid. Note: The perchloric acid must be washed clean to prevent it from drying out and collapsing during ashing. 1.4.7 Add 10 ml of perfluoric acid (1.2.4) to the filtrate and washing solution (1.4.6), and repeat the following analysis steps (1.4.5) to (1.4.6).
1.4.8 Place the two precipitates in original platinum, carefully dry and ash them, and place them in a muffle furnace to burn at 1000℃ for 30 minutes. Ministry of Chemical Industry of the People's Republic of China 1986-12-20 Issued 1987-09-01 Implementation
ZB D 51004-B6
Take them out, place them in a desiccator to cool to room temperature, weigh them, and repeat the burning until constant weight. 1.4.9 Use a small amount of water to moisten the precipitate, add 3-5 drops of sulfuric acid (1.2.5), 10m hydrofluoric acid (1.2.6), heat and evaporate until all white smoke is emitted, place the crucible in a muffle furnace and burn at 1000℃ for 30min, take it out, cool it to room temperature in a desiccator, weigh it, and repeat the burning until constant weight.
Carry out a blank test according to the entire analysis procedure. 1.5 Calculation of analysis results
The silicon dioxide (SiO2) content (X) is expressed as the mass fraction (%), calculated according to formula (1): Xi = (mi -m2) - (m3-ma)
The weight of the precipitate and platinum crucible before hydrofluoric acid treatment, 81 The weight of the precipitate and platinum crucible after hydrofluoric acid treatment, B! The weight of the reagent blank and platinum crucible before hydrofluoric acid treatment, g The weight of the reagent blank and platinum crucible after hydrofluoric acid treatment, g, each: one sample weight, g.
1.6 Tolerance
The tolerance of silicon dioxide in the parallel determination results of the wooden method is within 0.55% (absolute value), and the arithmetic mean of the parallel determination results is taken as the determination result.
2 Determination of silicon content in serpentine ore (potassium fluosilicate tolerance method) 2.1 Summary of the method
The sample is melted with sodium hydroxide flame, acidified by water leaching, potassium chloride and potassium chloride are added to the nitric acid solution to precipitate silicic acid in the form of potassium fluosilicate, filtered and washed to remove free acid, and the potassium fluosilicate precipitate is placed in boiling water for hydrolysis, and bromothymol blue-phenol red is used as an indicator, and the precipitated hydrochloric acid is titrated with sodium hydroxide standard solution. 2.2 Reagents
Sodium hydroxide (GB629-81).
Potassium nitrate (GB647--77)
Hydrochloric acid (GB 622-77): P1.19g/ml. Nitric acid (GB 626-78): 01.40 g/m 3. Hydroethanol (GB678-78): 95%. Potassium hydrogen phthalate (GB1257-77). Phenolic acid (HGB 3039-59): 0.5%. Potassium chloride (GB646-77): 25%. Potassium fluoride (GB1271-77). Potassium fluoride: 20%. Weigh 40 g of potassium fluoride (2.2.10) (KF: H20) and place it in a plastic cup. Add 150 ml of water and 2.2.11
50 ml of nitric acid (2.2.4). Add potassium chloride (2.2.8) to saturate. Let stand for 30 minutes. Filter with fast filter paper. Store the filtrate in a plastic bottle for later use.
Potassium nitrate and potassium fluoride washing solution: Weigh 5g potassium nitrate (2.2.2) and 2g potassium fluoride (2.2.10), place in a plastic beaker, 2.2.12
add 100ml water until dissolved (add a few drops of methyl red indicator, adjust to yellow with 5% sodium hydroxide and 1N hydrochloric acid). 2.2.13 Potassium chloride ethanol washing solution: Measure 50ml ethanol (2.2.5), add 50ml water, add potassium chloride (2.2.8) until saturated (add a few drops of methyl red indicator, adjust to yellow with 0.1N sodium hydroxide and 0.1N hydrochloric acid). 2.2.14 Methyl red: 0.5%. Weigh 0.5g methyl red, dissolve in 20ml ethanol (2.2.5), and dilute to 100ml with water. 2.2.15 Bromothymol blue phenol red indicator, weigh 0.09 g bromothymol blue and 0.11 g phenol red, dissolve in 20 ml ethanol (2.2.5) and 20 ml water, adjust to clear purple with 0.1 N sodium hydroxide, dilute to 100 ml with water (can be used for one month). ZBD51004-86
2.2.16 Sodium hydroxide standard solution: about 0.07 N, prepare sodium hydroxide (2.2.1) into a saturated solution, place in a plastic bottle, seal and place until the solution is clear, draw 3.7 ml of the clarified liquid, inject into a reagent bottle containing 1000 ml of water without carbon monoxide (pre-installed with a soda lime tube), and mix.
2.2.16.1 Calibration: Weigh 0.25-0.3g of potassium hydrogen phthalate (2.2.6) that has been dried at 105-110°C to constant weight, add 100ml of water to a 250ml beaker, heat and boil for 1min, quickly cool to room temperature, add 5 drops of phenol (2.2.7), and titrate with sodium hydroxide standard solution (2.2.16) until it turns pink as the end point. 2.2.16.2 Calculation: The equivalent concentration (N) of the sodium hydroxide standard solution is calculated according to formula (2): N=
0.2042 x V
Where: N—the equivalent concentration of the sodium hydroxide standard solution; m—the weight of the potassium hydrogen phthalate weighed in g;
—the volume of the sodium hydroxide standard solution consumed during titration, m1, 0.2042—the milligram equivalent of potassium hydrogen phthalate. 2.3 Sample
The sample is passed through a 106μm sieve and dried at 105-110℃ in a constant temperature desiccator. 2.4 Analysis steps
2.4.1 Weigh 0.58 of the sample (accurate to 0.00028), place it in a silver crucible covered with 3% sodium hydroxide (2.2.1), cover with 38% sodium hydroxide (2.2.1), cover (leave a gap), place the crucible in a muffle furnace, slowly heat to 750°C, melt for 30 minutes, take out and cool slightly, place in a 250ml plastic cup (10ml of water has been added to the cup in advance), add 80ml of boiling water, quickly cover the surface with blood, wait until the intense action stops, wash the crucible with hot water and dilute hydrochloric acid, quickly add 25ml of hydrochloric acid (2.2.3) while stirring until the solution is clear (to prevent silica agglomeration, hydrochloric acid should be added quickly at one time), after cooling, transfer to a 250ml volumetric flask, dilute to the scale with water, and shake to hook. 2.4.2 Take 25 ml of the test solution (2.4.1) and place it in a 250 ml plastic cup. Add 15 ml of potassium chloride solution (2.2.9) and 10 ml of nitric acid (2.2.4). Add 10 ml of potassium fluoride solution (2.2.11) while stirring. Continue stirring for 1 min. Let the precipitate sit for more than 20 min (preferably 2 to 4 h).
Positive: The amount of potassium fluorosilicate precipitation bath liquid should be controlled within 70 ml. The precipitation, washing and temperature should be controlled below 35. 2.4.3 Filter with a plastic funnel or waxed glass. Wash the plastic cup and funnel with potassium nitrate-potassium fluoride washing solution (2.2.12) until the washing solution retains its color (about 10 times): then wash 2 to 3 times with potassium chloride ethanol washing solution (2.2.13). : Filtration and washing operation, cut a piece of 2.5cm diameter filter paper, put it on a plastic funnel or a fine-pored porcelain plate coated with wax (fine-pored porcelain plate coated with wax, pierced with holes), start the pump, add filter paper pulp, wash 1 to 2 times with potassium amine ethanol washing solution (2.2.13), and then filter the test solution and precipitate by evacuation (one pump every time you wash). 2.4.4 Transfer the precipitate and the paper pulp into a plastic cup, add 10ml (2.2.13) solution, 12 to 10ml bromophenol blue-phenol red indicator (2.2.15). 5 drops, neutralize with sodium hydroxide standard solution until it turns stable purple (do not record the reading), add 150㎡1 of neutral boiling water, and titrate with sodium hydroxide standard solution until the solution turns bright purple as the end point. Perform a blank test according to the entire analytical procedure. Note: Add a few drops of indicator (2.2.15) to the neutral boiling water and adjust it to purple with sodium hydroxide (2.2.16). 2.5 Calculation of analytical results
The silicon monoxide (Sij02) content (X2) is expressed as mass white fraction (%), calculated according to formula (3): X2 =--(Vi-Vo) N × 0.01502
Wherein: V--
The volume of sodium hydroxide standard solution consumed by the test solution, m", X 100
The volume of sodium hydroxide standard solution consumed by the empty solution, mlThe equivalent concentration of sodium hydroxide standard solution: mg equivalent of silicon dioxide;
(3)
ZBD5100488
Take aliquots of the test solution equivalent to the weight of the sample, more. 2.6 Tolerance
The tolerance value of silicon dioxide in the downstream determination of this method is within D.55% (absolute value), and the arithmetic mean of the parallel determination results is taken as the determination result.
3 Determination of calcium and magnesium content in serpentine ore (EDTA volumetric method) This method refers to the ISO 6233—1983 "Manganese ores and concentrates—Determination of calcium and magnesium content—EDTA volumetric method". 9.1 Summary of the method
The sample is melted with sodium hydroxide, and iron, aluminum, manganese and other elements are separated with hexamethylenetetramine and sodium monoethyldithiocarbamate. In a strong alkaline medium, calcium is titrated with EDTA, and in an ammonia buffer medium, the calcium and magnesium are titrated with EDTA. 3.2 Reagents
Sodium hydroxide (GB629—81).
Hydrochloric acid (GB 62277): p1.19g/ml. Hydrochloric acid: 1+1.
Ammonia water (GB 631—77): e0.90g/ml (1 + 1). Hexamethylenetetramine.
Sodium-ethyl-thiocarbamate (copper reagent) (HG3—962—76). =Z Alcoholamine: 1 + 4.
Potassium hydroxide (GB2306-80): 20%. Dextrin: 4%. Weigh 4 dextrin, mix with water to make a paste, add 100ml boiling water. Ammonium chloride (GB 658-77).
Ammonia buffer solution, weigh 67.5ml ammonium chloride (3.2.10) and dissolve in water, add 570ml ammonia water (3.2.4), dilute with water to 1000ml, shake.
Acid chrome blue K: 0.5%.
Phenol green B: 0.5%.
Calcium oxide standard solution: 0.01000M. Weigh 1.0009g of standard calcium carbonate dried at 110-120℃, place in a 250ml8.2.14±
beaker, add 20ml water, slowly add 10ml hydrochloric acid (3.2.3) until dissolved, heat to a slight boil to remove carbon dioxide, cool, transfer to a 1000ml volumetric flask, dilute to scale with water, and shake. 8.2.15 Magnesium oxide standard solution: 0.0200M. Weigh 0.8060g of standard magnesium oxide burned to constant weight at 1000℃, place in a 250ml beaker, add 20ml water, slowly add 20ml hydrochloric acid (3.2.3), heat to dissolve, cool, transfer to a 1000㎡l volumetric flask, dilute to scale with water, and shake.
8.2.16 Disodium ethylenediaminetetraacetate (EDTA) (GB1401-78): 0.02M. Weigh 7.5g EDTA and dissolve it in water, dilute to 1000ml, and shake well.
3.2.16.1 Calibration: Pipette 20.00ml calcium oxide standard solution (3.2.14) and place it in a 250ml beaker, add 3-5ml magnesium oxide standard solution (3.2.15), and titrate with EDTA solution (3.2.16) according to the analysis steps (3.4.4), and titrate the blank solution at the same time.
Pipette 20.00ml magnesium oxide standard solution (3.2.15) and place it in a 250ml beaker, and titrate with EDTA solution (3.2.16) according to the analysis steps (3.4.5), and titrate the blank solution at the same time. Note: EDTA solution can also be calibrated with zinc standard reagent. 3.2.16.2 Calculate the molar concentration (M) of the BDTA standard solution according to formula (4): M - (v-Vo) where 1 is the molar concentration of the magnesium or calcium standard solution, M, (4) ZBD 5100486 is the volume of the magnesium or calcium standard solution pipetted, ml, V is the volume of the EDTA standard solution consumed during titration, m2!, and V is the volume of the EDTA standard solution consumed during titration of the blank solution, m2!. 3.3 Test sample The test sample shall be passed through a 106 μm sieve, dried at 105-110°C to constant weight, and placed in a desiccator. 3.4 Analysis steps
3.4.1 Weigh 0.2g of sample (accurate to 0.00028), place in a silver crucible covered with 28% sodium hydroxide (3.2.1), cover with 2g sodium hydroxide (3.2.1), cover the crucible with a lid (leave a gap), place in a muffle furnace, slowly heat to 750℃, melt for 30min. Take out and cool slightly, place in a 250ml beaker, add 50~60ml boiling water, quickly cover with blood on the surface, wait until the intense reaction stops, wash the crucible with hot water and dilute hydrochloric acid, add 10~15ml hydrochloric acid (3.2.2) until the solution is clear. 3.4.2 Add hydrogenated water (3.2.4) drop by drop until a precipitate appears, immediately add hydrochloric acid (3.2.3) until the precipitate dissolves, add 2g hexamethylenetetramine (3.2.5), stir evenly, add 0.1~0.2g copper reagent (3.2.6), stir evenly. 3.4.3 Transfer to a 25 ml container, dilute to the mark with water, shake, let stand to clarify, dry filter with medium-speed filter paper, and discard the initial filter blanket.
3.4.4 Determination of calcium oxide, transfer 50 ml of filtrate (3.4.3), place in a 250 ml beaker, add about 50 ml of water, 20 ml of dextrin solution (3.2.9), 5 ml of triethanolamine solution (3.2.7), stir, add 15 ml of potassium hydroxide solution (3.2.8), make the solution pH>12.5, add 2 drops of acid chrome blue K (3.2.12), 5 drops of naphthol green B (3.2.13), and titrate with EDTA standard solution (3.2.16) until the solution turns bright blue as the end point, and titrate the reagent blank solution at the same time. 3.4.5 Determination of magnesium oxide and calcium oxide content: Take 50 ml of the filtrate (3.4.3), place it in a 250 ml beaker, add about 100 ml of water, 5 ml of triethanolamine solution (3.2.7), stir well, add 10 ml of ammonia buffer solution (3.2.11) 2 drops of acid chrome blue K (3.2.12) and 6-7 drops of naphthol green B (3.2.13) are titrated with EDTA standard solution (3.2.16) until the solution turns bright green. At the same time, titrate the reagent blank solution.
Note: ① When the air humidity is below 15℃, the solution needs to be warmed to about 30℃ during titration. The complexation reaction proceeds normally. ② Acid storage monitor K and quinoa green B are different in quality, and their ratio can be appropriately adjusted to make the titration end point obvious. 3.5 Calculation of analysis results
3.5.1 Calcium oxide (CaO) content (X,) is expressed as mass percentage (%) and calculated according to formula (5): X; =M(Vi-Von) × 0.05608-x 100-the molar concentration of EDTA standard solution, M, where: M
The volume of EDTA standard solution consumed by calcium oxide in the test solution, ml, V
The volume of EDTA standard solution consumed by calcium oxide blank solution, ml1 Each liter of BDTA standard solution is equivalent to the number of grams of calcium oxide; The sample solution is equivalent to the sample weight, g. 3.5.2 Magnesium oxide (Mg0) content (X.) is expressed as mass percentage (%) and calculated according to formula (6): (5)
M ( (V2-Vo2) - (Vi-Vo1) 1 ×0.04030_ ×100 - (6) In the formula, the molar concentration of MEDTA standard solution, M, the volume of EDTA standard solution consumed by the calcium and magnesium content in the test solution, m1, K
0. 04 03 0
the volume of EDTA standard solution consumed by the blank solution of calcium and magnesium content, m1, each milliliter of EDTA standard solution is equivalent to the number of grams of magnesium oxide: one part of the sample solution is equivalent to the sample weight, star. 3. Tolerance
The allowable error of magnesium oxide in the half-measurement result of this prescription is within 0.40% (absolute value), and the arithmetic mean of the parallel measurement results is taken as ZBD51004-86
as the measurement result. When the calcium oxide content is less than 1%, the allowable error is within 0.15% (absolute value); when the content is greater than 1%, the allowable error is within 0.20% absolute value. The arithmetic mean of the parallel determination results is taken as the determination result. Determination of iron content in serpentine ore (titanium trifluoride-potassium dichromate titration) 4.1 Summary of the method
The sample is acidified with sodium hydroxide and molten hydrochloric acid. Most of the trivalent iron is reduced with tin nitride in a hydrochloric acid medium. In the presence of phosphotungstic acid, methyl orange is used as an indicator, and titanium trinitride is used to reduce the remaining trivalent iron. Sodium diamine sulfonate is used as an indicator to titrate with potassium dichromate standard paint solution.
4.2 Reagents
Sodium hydroxide (GB629-~81),
Hydrochloric acid (GB 622-77): 01.19g/m1. Hydrochloric acid 1 + 4.
Sulfuric acid (GB 625-77) → p1. 84g/ml. Phosphoric acid (GB1282-77) P1.70g/ml. Phosphoric acid: 5 + 95.
Sulfur-phosphorus mixed acid: slowly add 150ml sulfuric acid (4.2.4) into 700ml water, add 150ml phosphoric acid (4.2.5) after cooling, and stir.
4.2.8 Stannous fluoride (GB638-78), 5%. Weigh 58 stannous chloride, dissolve in 20m】hydrochloric acid (4.2.2) and dilute to 100ml with water, and store in a brown bottle.
Sodium phosphotungstate: 10%. Weigh 10 sodium tungstate and dissolve in 100m|phosphoric acid (4.2.6) 1. Titanium trichloride (HGB3122-59), 15-20% (1+100). Measure 1 ml of titanium trifluoride and 100 ml of hydrochloric acid 4.2.10 (4.2.3) and mix well. Methyl orange (HGB:3089-59): 0.1%. Potassium permanganate (GB 643--77) 0.5%.
Sodium diphenylamine sulfonate: 0.5%. Weigh 0.5 g of sodium diphenylamine sulfonate, dissolve in 100 ml of water, add 1-2 drops of sulfuric acid (4.2.4) and stir well.
Ferrous ammonium sulfate (GB661-77), 0.01N. Weigh 3.92 g of ferrous ammonium sulfate [FeSO4 (NH4) 2SO4 6Hz0) in a beaker, dissolve with a small amount of water, add 10 drops of sulfuric acid (4.2.4), transfer to a 1000 ml container, dilute with water to the mark, shake
Potassium dichromate (GB1259-77): standard reagent. 4.2.15
4.2.16 Potassium dichromate standard solution: 0.01000N. Weigh 0.4903g of potassium dichromate (4.2.15) dried at 150℃ for 1h and cooled to room temperature, dissolve it in a beaker with a small amount of water, transfer it to a 1000ml volumetric flask, dilute it to the scale with water, and shake it well. 4.3 Test sample
The test sample should pass through a 106um sieve, dry it at 105~110℃ until constant temperature, and place it in the lower desiccator. 4. 4 Analysis steps
4.4.1 Weigh 0.58g of the sample (accurate to 0.0002g), place it in a silver crucible with 38g of sodium hydroxide (4.2.1), cover it with 3g of sodium hydride (4.2.1), cover the crucible with a lid (leave a gap), place it in a muffle furnace, slowly heat it to 750℃ and melt it for 30min. Take it out and cool it slightly, place it in a 250ml beaker, add 50-60ml of boiling water, quickly cover it with a surface band, and after the intense reaction stops, wash the crucible with hot water and dilute hydrochloric acid, add 20ml of hydrochloric acid (4.2.2) until the solution is clear, transfer it to a 250ml volumetric flask, dilute it to the scale with water, and shake it. 4.4.2 Transfer 50ml of the test solution (4.4.1) to a 250ml beaker, heat and concentrate it to 30ml, add 10ml hydrochloric acid (4.2.2), remove and add stannous chloride (4.2.8) until the solution turns light yellow (if stannous chloride is added, potassium permanganate (4.2.12) can be added to make the solution turn light yellow again), dilute to 60ml with water, control the solution humidity at 30-60℃, add 10 drops of sodium phosphotungstate (4.2.9), add 1 drop of methyl orange solution (4.2.11), add titanium chloride solution (4.2.10), and change from red to colorless, and dilute the solution to 100ml. 4.4.3 Immediately add 10ml sulfur-phosphorus mixed acid (1.2.7), two drops of sodium diphenylamine sulfonate solution (4.2.13), and titrate with potassium dichromate standard solution (4.2.16) until the end point is stable purple. ZB D. 51004--86
Let: () When the reduction is close to the end point, the titanium trifluoride solution (4.2.10) should be added slowly to avoid excessive addition. If it is excessive, potassium dichromate standard solution (4.2.16) can be added dropwise to partially oxidize the iron, and then 1 drop of methyl chromate solution (4.2.11) can be added. Then, the titanium trifluoride solution will turn from red to colorless. ② After the trivalent iron is reduced, the standing time should not be too long, and it should be titrated with potassium dichromate standard solution within 5 minutes. 4.4.4 Blank determination: When operating with the sample, do not use stannous chloride during the reduction of the instrument. After adding sulfuric acid and phosphorus mixed acid, add 5 ml of ammonium ferrous sulfate (4.2.14), one drop of sodium phenylammonium sulfonate (4.2.13), and titrate with potassium dichromate standard solution (4.2.16) until the purple color is the end point. The number of milliliters of potassium dichromate standard solution consumed is A. Then add 5 ml of ammonium ferrous sulfate solution and titrate with potassium dichromate standard solution. The number of milliliters consumed is B. The number of milliliters of potassium dichromate standard solution consumed by the blank sample is Y. =AB. 4, 5 Calculation of analysis results
The content of trihydride iron (FerO) (X7) is expressed as mass percentage (%) and is calculated according to formula (7): X, - V-Vo) xN 0.07985-x100..-Book
In the formula. V.
The volume of potassium dichromate standard solution consumed by the test solution, m1, V. ---The volume of potassium dichromate standard solution consumed by the blank solution, m1N
The equivalent concentration of potassium dichromate standard solution, m
The test solution is equivalent to the weight of the sample, m, milligram equivalent of ferric oxide.
4.6 Tolerance
The allowable difference of ferric oxide in the parallel determination results of the method is within 0.25% (absolute value), and the arithmetic mean of the evaluation results is taken as the determination result.
B Determination of aluminum content in serpentine ore (EDTA tolerance method) This method refers to IS01169-1975 "Determination of aluminum content in zinc alloys". 5.1 Method Summary
The sample is acidified with alkaline molten hydrochloric acid, and hexamethylenetetramine is used to separate iron and tin from a large amount of magnesium into hydrogenated amine precipitation. The precipitation is dissolved with hydrochloric acid to remove iron, aluminum, etc. in the precipitation, and part of the silicon is removed. Excess EDTA is added to complex aluminum and other elements. The excess EDTA is titrated with zinc standard solution at pH 5.5-6 using monocresol orange as an indicator. Sodium fluoride is added to displace the EDTA complexed with aluminum, and the solution is titrated with zinc standard solution. 5.2 Reagents
Sodium hydroxide (GB 629—81)
Sodium hydroxide: 20%;
Sodium fluoride (GB1264—77)
Hydrochloric acid (GB 622-77): p1.19g/mi
Hydrochloric acid: 1+1
Hydrochloric acid: 1+3
Hydrochloric acid: 2+98;
Ammonia water (GB 631—77): p0.90g/m1 (1+1) Glacial acetic acid (GB 676—78): p1.05g/ml, glacial acetic acid, 1 +1
Sodium acetate (GB693-77)
Hexamethyltetramine: 20%;
Ammonium chloride (GB658-77) 1
Ammonium chloride washing solution, 2g ammonium chloride (5.2.13) dissolved in 100ml water 1, add 2-3 drops of ammonia (5.2.8) + acetic acid-sodium acetate buffer solution (pH~6): weigh 260g sodium acetate (5.2.11) (NaC2H3O2: 3Hz0) dissolved in 500ml water, add 10ml glacial acetic acid (5.2.9) and dilute with water to 100uml, ZB D 51004-86
5.2.16 Disodium ethylenediaminetetraacetate (EDTA) (GB1401-78): about 0.02M, 5.2.17 Anhydrous ethanol (GB 678-78) ;5.2.18
Cresol orange: 0.2%. Weigh 0.2g of cresol orange and dissolve it in 20ml of water, add 80ml of ethanol (5.2.17), shake and store in a brown bottle;
6.2.19 Congo red test paper,
Potassium ferrocyanide: 5%;
Aluminum sheet (99.99%)
5.2.22 Aluminum standard solution: 0.0100M. Weigh 0.2698g of aluminum sheet (5.2.21), place it in a polytetrafluoroethylene beaker, add 10ml of sodium hydroxide (5.2.2), dissolve it in warm water, then add 20ml of hydrochloric acid (5.2.5), heat until the solution is clear, cool, transfer to a 1000ml container, dilute to the scale with water, shake well, 5.2.23 Zinc acetate (HG 3-1098-77): about 0.01M 5.2.23.1 Preparation Weigh 2.2 ml of zinc acetate [Zn (CH,C00)2*2H20] and dissolve it in water, add 2ml of glacial acetic acid (5.2.9), dilute to 1000ml with water, and shake well.
5.2.23.2 Calibration: Pipette 20ml of aluminum standard solution (5.2.22) into a 250ml beaker, dilute to 100ml with water, add 15ml EDTA (4.2.16) and proceed according to analysis steps 4.4.4 to 4,4.5. 5.2.23.3 The molar concentration M of zinc acetate solution is calculated according to formula (8): M =
Where: M,-
Mr· Y
The molar concentration of aluminum standard solution, M:
The volume of aluminum standard solution transferred, m!,
The volume of zinc acetate solution consumed during titration, m1. 5.8 Sample
The sample is passed through a 106um sieve, dried at 105~110℃ to constant weight, and placed in a card desiccator. 5.4 Analysis steps
5.4.1 Weigh 0.2% of the sample (accurate to 0.00028), place it in a silver crucible covered with 28% sodium hydroxide (5.2.1), cover it with 28% sodium hydroxide (5.2.1), cover it with a lid (leave a gap), place it in a muffle furnace and slowly heat it to 750℃, melt it for 30 minutes, take it out and cool it slightly, place it in a 250ml beaker, add 50-60ml boiling water, quickly cover it with a watch glass, wait until the intense action stops, wash out the crucible with hot water and dilute hydrochloric acid, add 10-15ml hydrochloric acid (5.2.4) until the solution is clear. 5.4.2 Heat the solution to boiling, add 18% ammonium chloride (5.2.13) and neutralize with nitrogen water (5.2.8) until the precipitate just appears, immediately add hydrochloric acid (5.2.5) until the precipitate dissolves, slowly add 20ml hexamethylenetetramine solution (5.2.12) under stirring, heat to boiling and remove, wait for the precipitate to condense, filter with rapid quantitative filter paper while hot, wash the beaker and precipitate twice with hot ammonium oxide washing solution (5.2.14). 5.4.3 Use about 30ml hot hydrochloric acid (5.2.5) to rinse the precipitate, take the solution with the original burning forest, and wash with hot dilute hydrochloric acid (5.2.7) until the ferric iron (check with potassium ferrocyanide solution (5.2.20)) 1 Control the volume of the solution to 100-150ml. 6.4.4 Add 1015ml EDTA solution (5.2.16) (the amount should be sufficient to completely complex the iron and aluminum ions in the solution and the excess should be 3~5㎡l), add a small piece of Congo red test paper (5.2.19), add ammonia water (5.2.8) to neutralize until the test paper turns red, add 10ml acetic acid-sodium acetate buffer solution (5.2.15), heat and boil for 2 minutes, remove and cool to room temperature, add 4~5 drops of xylenol orange solution (5.2.18), and titrate with zinc acetate standard solution (5.2.23) until the solution turns slightly red (ignore the reading). 6.4.6 Add 0.5g sodium fluoride (5.2.3) and stir, boil for 2~3 minutes, remove and cool to room temperature, add 1~2 drops of xylenol orange (5.2.18), and titrate with zinc acetate standard solution (5.2.23) until the solution turns slightly red as the end point, and perform a blank test according to the entire analytical steps. 5.5 Calculation of analysis results
The content of aluminum oxide (A1203) (X,) is expressed as mass percentage (%) and is calculated according to formula (9): ZB D 51004-88
Xg = M (V-Vo) ×0.05098×100 -m
Wherein: M—molar concentration of zinc acetate standard solution, M; volume of zinc acetate standard solution consumed by the test solution. Work! , Vo—volume of zinc acetate standard solution consumed by the blank solution, m1—weight of the sample, g;
0.05098—grams of aluminum oxide equivalent to each milliliter of zinc acetate standard solution. Note: The determination result of this method is aluminum titanium content, and the serpentine titanium content is ≤0.001%. (9)
5.6 Tolerance
When the content of aluminum oxide in the parallel determination results of this method is less than 1%, the tolerance is within 0.1% (absolute value); when the content is greater than 1%, the tolerance is within 0.15% (absolute value). The arithmetic mean of the parallel determination results is taken as the determination result. 6 Determination of nickel content in serpentine ore ("diketone oxime photometric method) 6.1 Summary of the method
The sample is decomposed with aqua regia and sulfuric acid, potassium sodium tartrate is used as a masking agent, and nickel and diacetyl form a wine-red complex in an ammonia solution with an oxidant, and its absorbance is measured. 8.2 Reagents
Hydrochloric acid (GB622-77): Pl.19g/ml
Nitric acid (GB626-78): p1.40g/ml
Sulfuric acid (GB625-77): p1.84g/ml (1+1), 6.2.8
Sodium potassium bisphenol A (GB1288-77) 120%6.2.4
6.2.5Ammonium persulfate (GB 655-77): 5% (prepare when used)sSodium hydroxide (GB629-81): 5%
Diacetyl: 1%. Weigh 1g of diacetyl and dissolve it in 100ml of sodium hydroxide solution (6.2.6) → 6.2.8 Hydrogen water (GB 631-77): p0.90.g/ml, (1 +1) 6.2.9 Potassium fluoride (GB1271--77).
6.2.10 Nickel oxide standard solution:
6.2.10.1 Preparation: Weigh 1.0000g of nickel oxide (spectrally pure) in a 100ml beaker, add 25ml of hydrochloric acid (6.2.1), cover with a watch glass, heat at low temperature until completely dissolved, cool and dilute to 1000m] with water, shake, this solution contains 1Ⅲ nickel oxide per ml. 6.2.10.2 Take 50 ml of nickel standard solution (6.2.10.1) and place it in a 500 ml volumetric flask, dilute it to the mark with water, and add a spoon. This solution contains 1004 g of nickel oxide per ml. wwW.bzxz.Net
6.2.10.3 Take 50 ml of nickel standard solution (6.2.10.2) and place it in a 500 ml volumetric flask, dilute it to the mark with water, and add a spoon. This solution contains 10 ug of nickel oxide per ml.
6.3 Sample
The sample is passed through a 106 um sieve, dried at 105 to 110°C to constant weight, and placed in a desiccator. 6.4 Analysis steps
6.4.1 Weigh 0.2g of sample (accurate to 0.0002g) and place it in a 200ml polytetrafluoroethylene beaker. Add 10ml hydrochloric acid (6.2.1), 3ml nitric acid (6.2.2) and 0.58 potassium fluoride (6.2.9). Heat on a hot plate to dissolve and evaporate to nearly ten. Add 5ml of sodium pyrochlore (6.2.3) Heat until white smoke appears for 3-5 minutes, and cool. Add 301 water and boil to dissolve all soluble salts, transfer to a 100ml volumetric flask, dilute with water to 1/3, shake well, filter, and discard the initial filter. 6.4.2 Transfer 2 portions of the 10ml filtrate (6.4.1) and place them in 50ml volumetric flasks respectively, and perform analysis according to steps 6.4.3 and 16.4.4 respectively. 6.4.3 Color developing solution: Add 10ml potassium sodium tartrate solution (6.2.4) and neutralize with ammonia water (6.2.8) until the yellow color of the test solution begins to disappear, then add 2ml excess, add 10ml ammonium persulfate (6.2.5), immediately add 5ml diacetyl (6.2.7), dilute with water to the mark, and shake well. Let stand for 15-20 minutes.
ZBD 51004-86
6.4.4 Reference solution, add 10ml potassium sodium tartrate solution (6.2.4), neutralize with ammonia water (6.2.8) until the yellow color of the test piece begins to disappear, then add 2ml excess, add 10ml ammonium persulfate (6.2.5), dilute with water to the scale, and shake well. .4.5 Transfer solutions 6.4.3 and 6.4.4 into 1cm colorimetric blood, use reference solution (6.4.4) as reference, measure its absorbance at a wavelength of 530mm, and find the corresponding nickel content on the working curve. 6.5 Drawing of working curve
Pipette 0.00, 2.00, 4.00, 6.00, 8.00, 10.00 ml of nickel oxide standard solution (6.2.10.3) and place them in 6 50 ml volumetric flasks respectively. Perform the analysis according to (6.4.3). Then measure the absorbance according to (6.4.5). Draw the working curve with the absorbance as the ordinate and the corresponding nickel content as the abscissa. 6.6 Calculation of analysis results
The nickel oxide (NiO) content (X10) is expressed as mass percentage (%) and is calculated according to formula (10): X =
where tc
c×102×100
is the nickel oxide content obtained from the working curve F, μB; take a test solution equivalent to the weight of the sample, 8.
6.7 Tolerance
The tolerance of nickel oxide in the parallel determination results of this method is within 0.03% (absolute value). The arithmetic mean of the parallel determination results is taken as the determination result.
T Determination of ignition loss of serpentine ore (gravimetric method) 7.1 Summary of the method
The sample is placed in a muffle furnace and burned at 950℃ until constant weight. The ignition loss is calculated based on the lost weight. 7.2 Sample
The sample is passed through a 106μm sieve, dried at 105~110℃ until constant weight, and placed in a desiccator. 7.3 Analysis steps
Weigh 1.00g of the sample and place it in a porcelain worm that has been burned to constant weight, place it in a muffle furnace, gradually increase the temperature to 950℃ and burn for 11.5h, take it out, cool it slightly, place it in a desiccator to cool to room temperature and weigh it, and burn it repeatedly until constant weight (the second burning time is 30min). 7.4 Calculation of analysis results
Ignition loss (X1) is expressed as mass percentage (%) and is calculated according to formula (11): X
In the formula, m-
weight of sample and crucible before ignition, B
weight of sample and crucible after ignition,
weight of sample,
m1—m2
T.5 Tolerance
The maximum tolerable difference of ignition loss of parallel determination results of this method is within 0.30% (absolute value). The arithmetic mean of the parallel determination results is taken as the determination result.
Determination of adsorbed water content of serpentine ore (gravimetric method) 8.1 Summary of the method
Weigh 1000g of a sample with a diameter less than [cm, dry it at 105-110℃, and calculate the adsorbed water content based on the weight loss. 3.2 Instruments and apparatus
8.2.1 Balance, weighing up to 2000g, sensitivity 1g8.2.2 Drying oven: with automatic temperature controller. 8.2.3 Sample container: porcelain plate.
8.3 Sample
Sample particle size: less than 1cm in diameter.
ZB D 51004—86
8.4 Analysis steps
Weigh 1000g of sample (accurate to 18) and spread it evenly on a porcelain plate with a known weight, place it in an oven at 105-110℃ and dry it for 2h (after drying for 1h, gently stir it with a glass rod). Take it out and cool it down, then weigh it again after drying, until the difference between the two weighings is no more than 28. B.5 Calculation of analysis results
The adsorbed water content (X2) is expressed as a percentage of mass (%) and is calculated according to formula (12):X
In the formula, Gi is the weight of the sample and the porcelain plate before drying, G2 is the weight of the sample and the porcelain plate after drying, g; m is the weight of the sample, 8.
BB Tolerance
The tolerance of the parallel determination results of this method is within 0.15% (absolute value), and the arithmetic mean of the determination results is taken as the determination result.
Additional explanation,
This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China and is under the jurisdiction of the Chemical Industry Design and Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Chemical Industry Design and Research Institute. The main drafters of this standard are Li Fengdie, Shi Jiming, Zhu Jingjuan, and Man Lin.3 Sample container: porcelain plate.
8.3 Sample
Sample particle size: less than 1 cm in diameter.
ZB D 51004—86
8.4 Analysis steps
Weigh 1000 g of sample (accurate to 18) and spread it evenly on a porcelain plate with a known weight, place it in an oven at 105-110℃ for 2 hours (after drying for 1 hour, gently stir it with a glass rod). Take it out and weigh it after cooling, and then dry and weigh it again until the difference between the two weighings is no more than 28. B.5 Calculation of analysis results
The adsorbed water mouse (X2) is expressed as a percentage of the mass disk (%) and is calculated according to formula (12): X
In the formula, Gi is the weight of the sample and porcelain plate before drying, G2 is the weight of the sample and porcelain plate after drying, g; m is the weight of the sample, 8.
BB Customer Tolerance
The allowable difference of the parallel determination results of this method is within 0.15% (absolute value), and the arithmetic mean of the determination results is taken as the determination result.
Additional explanation,
This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China and is under the jurisdiction of the Chemical Industry Design and Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Chemical Industry Design and Research Institute. The main drafters of this standard are Li Fengdie, Shi Jiming, Zhu Jingjuan, and Man Lin.3 Sample container: porcelain plate.
8.3 Sample
Sample particle size: less than 1 cm in diameter.
ZB D 51004—86
8.4 Analysis steps
Weigh 1000 g of sample (accurate to 18) and spread it evenly on a porcelain plate with a known weight, place it in an oven at 105-110℃ for 2 hours (after drying for 1 hour, gently stir it with a glass rod). Take it out and weigh it after cooling, and then dry and weigh it again until the difference between the two weighings is no more than 28. B.5 Calculation of analysis results
The adsorbed water mouse (X2) is expressed as a percentage of the mass disk (%) and is calculated according to formula (12): X
In the formula, Gi is the weight of the sample and porcelain plate before drying, G2 is the weight of the sample and porcelain plate after drying, g; m is the weight of the sample, 8.
BB Customer Tolerance
The allowable difference of the parallel determination results of this method is within 0.15% (absolute value), and the arithmetic mean of the determination results is taken as the determination result.
Additional explanation,
This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China and is under the jurisdiction of the Chemical Industry Design and Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Chemical Industry Design and Research Institute. The main drafters of this standard are Li Fengdie, Shi Jiming, Zhu Jingjuan, and Man Lin.
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