HG/T 2271.2-1992 Test method for platinum catalyst for S201 nitric acid production
Some standard content:
Chemical Industry Standard of the People's Republic of China
HG 2271. 1 92
HG/T2271.2-92
Platinum catalyst for S201 nitric acid production
and its test method
1992-03-03 Issued
Ministry of Chemical Industry of the People's Republic of China
Standards and Regulations Network wbzg口om Various standard industry materials free download 1993-01-01 implementation
HG2271.1—92S201 type nitric acid production platinum catalyst list||t t||HG/T2271.2—92Test method for platinum catalyst used in S201 nitric acid productionG77HG/T2430-93
Water treatment agent scale inhibitor Ⅱ
G77HG/T2431-93
Water treatment agent scale inhibitor class
1994-01-01
1994-01-01
Corrigendum to chemical standard HG/T2271.2-92 has been found, HG/T2 271.2-92 "Test Method for Platinum Catalyst for S201 Nitric Acid Production" has errors in its content. The corrections are as follows:
(1) The last line of 3.4, "Move into 25.00ml capacity", should be changed to "Move into 250ml container bottle", (2) 5.1, add "Take the arithmetic mean of three measurements as the measurement result" at the end, (3) 5.3, add "Take the arithmetic mean of each measurement as the measurement result". One sentence, standard specification network wmbzgoo-cm various Standard industry data free download Chemical industry standards of the People's Republic of China
Test method for platinum catalyst used in S201 nitric acid production 1 Subject content and scope of application
HG/T2271.2-92
This standard specifies the test methods for main elements, trace impurity elements, physical parameters, break joints and mesh defect areas of platinum catalyst used in S201 nitric acid production.
This standard is applicable to platinum catalyst used in S201 nitric acid production. 2 Reference standards||t t||GB6682 Laboratory Water Specifications
3 Determination of Main Elements
3.1 Principle
Palladium forms diacetyl palladium precipitate with diacetyl in hydrochloric acid medium, and the palladium content is determined by weighing method. The chloro complex of platinum, palladium and chalcopyrite is oxidized by sodium bromate, and then adjusted to pH 7.5~8.0 with sodium bicarbonate, so that palladium and chalcopyrite are separated from platinum in the form of hydrated oxide precipitation. In the slightly acidic solution of palladium and chalcopyrite chloro complex: add sodium nitrite and hexaammine nitrate complex cobalt (co) solution , so that the cobalt hexanitrite hexaamine complex salt precipitation is formed, and the cobalt content is determined by weighing method. When the percentage of palladium and total trace impurities is measured, the platinum content is obtained by subtraction method. 3.2 Reagents and solutions
3.2.1 Nitric acid (GB626);
3.2.2 Sodium nitrite (GB633);
3.2.3 Anhydrous ethanol (GB678);
3.2.4 Hydrochloric acid (GB622) solution;
3.2.4 .11+1 solution;
3.2.4.27% (V/V) solution;
3.2.5 Sodium fluoride (GB1266) solution;
3.2.5.1100g/L solution;
3.2.5.210g/L solution;
3.2.6 Butanedione (HG3-961) ethanol solution: 10g/L; Sodium bromate solution: 100g/L;
Sodium bicarbonate (GB640) solution: 1 00g/L; 3.2.8
Hexaamminechromium cobalt (III) nitrate solution (preparation method see Appendix A); 3.2.9
3.2.9.1 Hexaamminechromium cobalt (II) nitrate saturated solution (preparation method see Appendix A); 3.2.9.2 Hexaamminechromium cobalt nitrate 0.5g/L solution: 3.2.10 Dilute aqua regia: hydrochloric acid (3.2.4) + nitric acid (3.2.1) + water = 3+1+1. The water used for sample analysis should meet the third-grade water specifications in GB6682. 3.3 Instruments and Equipment
Approved by the Ministry of Chemical Industry of the People's Republic of China on March 3, 19924
Standard Authorization Network: w.bxtomh(con1993-01-01 Implementation
General analytical instruments in the laboratory;
Electric furnace with voltage regulator,
3.4 Preparation of test solution
HG/T2271.2-92
Weigh about 5g of the sample in the laboratory and place it in a 200mL beaker, add 50mL of hydrochloric acid (3.2.4.1) and boil for 10min to clean its surface. Then boil and wash it with water three times. Transfer the surface treated sample to a glass container, put it in an oven and bake it at 110C for 1h, then take it out and put it in a desiccator, and cool it to room temperature. Weigh about 2.5g (accurate to 0.0001g) of the treated sample in two portions, place them in 500mL beakers, add 50mL of dilute aqua regia (3.2.10), place on an electric stove with a voltage regulator and heat to near boiling until the sample is completely dissolved, continue heating to concentrate the dissolved volume to about 10mL, then add concentrated hydrochloric acid (10mL each time) (3.2.4) three times, evaporate to near dryness, add 35mL of sodium chloride solution (3.2.5.1), evaporate to near dryness. Remove and cool, dissolve in a small amount of water, transfer to a 25.00mL volumetric flask, dilute to the mark with water, mix well and set aside. 3.5 Determination of palladium
3.5.1 Determination procedure
Use a pipette to draw 100.00mL of the test solution and place it in a 50 0mL beaker, steam on an electric stove with a voltage regulator until almost dry, add 200mL hydrochloric acid solution (3.2.4.2) and slowly add 20mL of diacetyl ethanol solution (3.2.6) under stirring. After precipitation is complete, filter with a No. 4 quartz sand core funnel that has been dried to constant weight, wash with hydrochloric acid solution (3.2.4.2) until the filtrate is colorless; then wash with water until the filtrate is neutral. After draining the quartz sand core funnel, place it in an oven at 110℃ for 1h. Take it out and put it in a desiccator to cool for 0.5h and weigh it until constant weight,
3.5.2 Expression of analysis results
The mass percentage of palladium X is calculated according to formula (1): X,
Where: m is the mass of diacetyl palladium, g
m2—the mass of the sample, g;| |tt||m,×0.3161
Conversion coefficient of dibutyl acetone palladium to palladium,
3.5.3 Allowable difference
The difference between two parallel determination results should not be greater than 0.1%. Take the arithmetic mean as the determination result. 3.6 Determination
3.6.1 Determination procedure
Pipette 50.00mL of test solution and place it in a 500mL beaker. Place it on an electric stove with a voltage regulator and evaporate it to near dryness. Add 200mL of water, heat to boiling, adjust the pH to 1.5 with hydrochloric acid solution (3.2.4.1), add 25mL of sodium bromate solution (3.2.7) and boil for 30min, adjust the pH to 7.5~8.0 with sodium bicarbonate solution (3.2.8), and boil for 30min. Then remove and quickly cool to room temperature in a cold water bath. Filter with a No. 4 quartz sand core funnel and wash with a sodium chloride solution (3.2.5.2) with a pH of 7.0 until the filtrate is colorless. Add 25 mL of concentrated hydrochloric acid (3.2.4) to the precipitate in the funnel and leave for 1 hour. After the precipitate is completely dissolved, filter and wash with water until the filtrate is colorless. Put the filtrate into the original beaker and concentrate it to 1-2 mL on an electric furnace with a voltage regulator. Add 300 mL of water and heat to 60°C. Use a hydrochloric acid solution ( 3.2.4.1) to adjust the pH value to 1.5-3.0, add 5g sodium nitrite (3.2.2) and continue heating to a slight boil until the solution turns light yellow, stop heating, add 30ml saturated solution of hexaammine cobalt nitrate (3.2.9.1) under stirring, then accelerate stirring for 3-5min to allow all the precipitates to precipitate, immerse the beaker in cold water for 0.5h, and filter with a No. 4 quartz sand core funnel that has been dried to constant weight. The precipitate is first washed three times with hexaammine cobalt nitrate solution (3.2.9.2) (about 10 mL each time), and the precipitate is completely transferred to a No. 4 quartz sand core funnel. Finally, it is washed three times with 30 mL of anhydrous ethanol (3.2.3). The quartz sand core funnel is placed in an oven at 110°C for 0.5 h, then taken out and placed in a dryer for cooling and weighing until constant weight is obtained. 3.6.2 Expression of analysis results
The mass percentage content X is calculated according to formula (2): Standards Executive Network bm-ccn Various American Standard Industry Data Free Download In the formula: m
The mass of the double salt precipitate of armor, g:
The mass of the sample taken, g:
The conversion coefficient of the double salt of armor to the metal.
3.6.3 Allowable difference
HG/T 2271.2 -92
m.x0.1905
The difference between two parallel determination results should not be greater than 0.1%. The arithmetic mean is taken as the determination result. 3.7 Calculation of platinum content
The mass percentage content of platinum, X, is calculated according to formula (3): X, =-100 (X +X,+X)
Wherein: X, is the mass percentage content of palladium;
is the mass percentage content of niobium;
X.—The mass percentage content of total trace impurity elements. 4 Determination of trace impurity elements
4.1 Scope of application
The content range of impurity elements determined by this method is shown in Table 1. 1
Cu, Mg
Fe.Ni.Cr.Bi.Al,Pb
Ca,Zn
2 Principle
Determination range, %
0.0001~0.004
0. 000 512~0. 02
.00128~0.05
0.00255~0.1
（3）
Using a DC arc light source, the ions of various elements in the powdered platinum catalyst contained in the small hole of the cup-shaped graphite electrode are heated and vaporized and excited. When the atoms or ions in different excited states migrate back to lower energy levels, they radiate a spectrum with characteristic wavelengths. Select the wavelength spectrum of the element to be determined as the analysis line, measure the blackness of the harmonic edge to determine the intensity of the spectrum line, and compare it with the intensity of the corresponding spectrum line in the standard sample to determine the content of the filtered element: 4.3 Reagents and materials
4.3.1 Nitric acid (GB626): high-grade pure:
4.3.2 Hydrated difluoride (HGR3200):
4.3.3 Spectral pure graphite electrode: diameter 6mm; 4.3.4 Spectral photosensitive plate: Tianjin UV type 1; 4.3.5
Hydrochloric acid (GB622): high-grade pure:
4.3.6 Hydrochloric acid (high-grade pure) 1+1 solution; 4.3.7
Dilute aqua regia: hydrochloric acid (4.3.5) + nitric acid (4.3.1) + water = 3-1+1 The water used for analyzing the sample should meet the third-grade water specifications in GB5682. 6
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HG/T2271.2--92
Matrix composition: platinum (Pt) 93%, germanium (Rh) 4%, palladium (Pd) 3%, other impurity elements content see Table 2.4.5 Instruments and equipment
4.5.131W two-meter plane grating spectrometer; UBI-1 light source;
4 .5.3 Zeiss Type I microphotometer;
Spectral calculation board or PC-1500 computer and semi-automatic photometry system;4.5.4
4.5.5Electrode processing lathe;
4.5.6Tube electric furnace, quartz tube, quartz boat;4.5.7Agate grinding body;
Electric furnace with voltage regulator,
Note: Other types of instruments and equipment are allowed to be used under the premise of ensuring the precision and accuracy of analysis. The impurity content in the standard sample is shown in Table 2.
Content, %
Cu, Mg
Pb, Cr, Ni, Fe, Bi, Al
Ca, Zn
4.6 Preparation of samples
Sample number
Weigh about 0.25g of laboratory sample in 2 portions, place them in 100mL beakers respectively, add 20mL of hydrochloric acid solution (4.3.6), boil for 10min, pour out the liquid, and then boil and wash with water Three times (20 mL each time), add 20 mL of dilute aqua regia (4.3.7) and heat to dissolve (avoid boiling. After the solution is completely dissolved, evaporate to nearly dryness. Add 10 mL of hydrochloric acid (4.3.5) and evaporate to nearly dryness. Repeat the operation three times to drive out nitrogen dioxide, add 20 mL of water. Evaporate to nearly dryness again, repeat twice, add 20 mL of water, slowly add 3 mL of hydrated nitrogen (4.3.2) drop by drop, and stir quickly to precipitate completely. Move the solution and precipitate under an infrared lamp to dry. Grind the material into a fine mixture, transfer it to a quartz boat, place it in a tube furnace, raise the temperature to 200°C in an air atmosphere within 0.5h, keep the temperature constant for 0.5h, then continue to raise the temperature to 400°C, keep the temperature constant for 0.5h, cool the metal powder to room temperature and weigh it. Add spectrally pure graphite powder to make the ratio of metal powder to graphite powder equal to 4:1, grind it evenly and set it aside. 4.7 Measurement conditions
.7.1 Light source: UBI-1 light source. Working voltage: 300V: Working current: Leveled DC 7A.4.7.2 Spectrophotometry Instrument: 31WⅡ two-meter plane photoelectrode spectrograph. Grating lines 600 lines/mm: Gain gap: 10u; Light bar turntable three-valence ladder: middle light bar 2.5mm; Working center wavelength 3003×10-m7.3 Electrode: @6mm spectral pure graphite electrode, sample loading is 15~20mg, pole distance 3mm, electrode shape is shown in the figure below. Standard specification network wmbzgoo-cm various standard industry data free download 2
Lower electrode
HG/ T2271.2—92
Figure Electrode shape
Upper electrode
4.7.4 Photosensitive plate: Tianjin UV type 1, specification 9cm×24cm. 4.7.5 Exposure method: pre-burning time 0s, exposure time 80s, DC arc anode excitation, sample powder, graphite electrode pinhole spectrum.
4.7.6 Analysis line pair: The analysis line and its transmittance, the internal standard line and its transmittance, and the analysis line background measurement position are specified in Table 3. Table 3
Related regulations
Impurity elements
Development and fixing conditions
Transmittance
Backmost measurement
Perform according to the instructions of the photosensitive plate
10-10m
Transmittance
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10~1°m
Transmittance
HG/T2271.2-92
4.7.8 Photometric measurement: Use microphotometer S scale to measure 4.8 Operating procedures
Under the conditions of 4.7, the three-standard sample method is used. The standard samples (No. 1 to No. 5) and the tested samples are spectrally photographed and the photosensitive plates are processed on the same plate. Since different calculation tools are currently used in different laboratories, the operating procedures are described as follows: 4.8.1 Use of spectrum calculation board
4.8.1.1 Preparation of emulsion characteristic curve:
Before the batch of plates are used, the step dimmer method is used to prepare the emulsion characteristic curve of the batch of photosensitive plates. 4.8.1.2 Preparation of working curve:
A working curve must be prepared for each sample analysis. Use the microphotometer S scale to measure the photometry, and use the logarithm (logR) of the relative intensity of the analysis line of each impurity element in the standard sample (No. 1, No. 5) with the internal standard line after deducting the background as the vertical coordinate, and the logarithm (logC) of the corresponding percentage content of each impurity element as the horizontal coordinate to draw the working curve of each impurity element. 4.8.1.3 Expression of analysis results:
Use the logR of each impurity element in the tested sample to find the corresponding logC on its working curve, and then use the logarithmic table to convert the logC of each impurity element in the tested sample into percentage content (m/m). 4.8.2 Use PC-1500 computer and its semi-automatic photometry system. 4.8.2.1 Operation procedure Follow the computer operating instructions. 4.8.2.2 Expression of analysis results
Take the arithmetic mean of the two parallel results printed out by the printer as the measurement result , 4.9 Allowable difference
When the impurity content is <0.001% (i.e. 10×10-6), the relative error of the two parallel determination results is ≤100%: when the impurity content is between 0.001% and 0.015% (i.e. 10×10-~150×10~), the relative error of the two parallel determination results is ≤60% 5 Physical parameter determination method
5.1 Determination of wire diameter
Measured with an external micrometer caliper, the wire diameter is measured at no less than three points per tube, and the distance between any two measuring points shall not be less than 300mm. The wire diameter should be measured accurately to 0.001mm.
5.2 The tensile strength and elongation of the finished wire are measured using a single yarn strength machine of type Y361 with a tensile range of 0~1000CN, and 200mm is clamped for each finished wire. Fix the finished wire to be tested firmly on the upper and lower wire clamps, turn on the lifting handle to make the lower wire clamp descend at a uniform speed. After the wire breaks, the pointer of the strength machine and the extension ruler stop moving, record the tension and elongation values, and measure each tube three times. The tensile strength X of the wire (MPa) is calculated according to formula (4): X
Where: F strength reading, CN;
d wire diameter, mm;
0.01—CN conversion coefficient to N,
The elongation X of the wire (%) is calculated according to formula (5): F×0.01
Where: L,Wire extension length, mm;
200—Measured wire length, mm.
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5.3 Determination of mesh number
HG/T2271.2-92
Measure the mesh number with a fabric warp and weft density microscope. When the mesh diameter is not greater than 2070mm, the number of measuring points for each mesh shall not be less than three; when the mesh diameter is greater than 2070mm, the number of measuring points for each mesh shall not be less than six, and the distance between any two measuring points shall not be less than 300mm, and the connecting line shall not be consistent with the direction of the warp and weft wires
5.4 Determination of mesh diameter
Measure with a 10m long steel tape measure with a graduation value of 5mm. Each net is measured four times, once in the warp direction and once in the weft direction, and once in the 45° direction between the warp and weft. The average of the four measurements is taken as the net diameter measurement result. 5.5 Determination of the mass of net per square meter
5.5.1 Determination procedure
Weigh the mass of the net with a five-level balance with a maximum sample weight of 50kg and a sensitivity of 100mg, accurate to 0.1g. 5.5.2 Expression and calculation of results
The unit area mass X of the mesh (g/m2) is calculated according to formula (6): m
Yuan(D+0.02)
Wherein: ms
Mass of the mesh, g:
Diameter of a mesh, m;
Length of the joint of a mesh, m;
Number of joints of a mesh;
0.02——Total width of the edge of the mesh, m;
0.01Width of the joint of the mesh, m.
6 Determination of the number of breaks, joints and mesh defect area
+L.×0.01×A
6.1 Place the finished mesh on a glass mesh inspection table with lighting equipment underneath, and visually inspect the number of breaks and joints section by section. 6.2 Determination of mesh defect area
Measure with a fabric warp and weft density mirror and a 50cm steel ruler with a graduation value of 1mm. First visually check the location of the sparse and dense channels, horizontal wefts, and loose threads in the mesh surface, and then use the fabric warp and weft density mirror to determine whether the mesh holes are within the range of 961 to 1089 holes/cm2. If it is confirmed to be unqualified, measure its length and width with a steel ruler and calculate the mesh defect area. When measuring the mesh defect area, it should be accurate to 0.1cm210
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A1.1 Cobalt nitrate (Ⅱ);
A1.2 Ammonium nitrate (GB659);
A1.3 Ammonia water (GB631);
A1.4 Activated carbon (powder):
A1.5 Nitric acid (GB626);
HG/T 2271.2—92
Preparation of hexaammine cobalt (II) nitrate and its saturated solution (supplement)
A2 Preparation of hexaammine cobalt (III) nitrate Dissolve 73 g of cobalt (II) nitrate (A1.1) in 100 mL of water, add 80 g of ammonium nitrate (A1.2), 2 g of activated carbon (A1.4), and 100 mL of ammonia water (A1.3). After air is passed through the solution for 3 to 4 hours, add 1300 to 1500 mL of water acidified with 50 mL of nitric acid (A1.5), and heat on a water bath until the yellow precipitate is dissolved. Then filter the solution, remove the activated carbon, add 200 mL of nitric acid to the filtrate, and after cooling, an orange crystalline precipitate is precipitated. Filter it with a quartz sand core funnel, wash the precipitate with mother liquor and ethanol, dry it in an oven at 100°C, and store it in a ground-mouth bottle for later use. A3 Preparation of saturated solution of hexaammine cobalt nitrate (II) Weigh 17g of hexaammine cobalt nitrate (II) prepared according to Chapter A2, dissolve in 200mL hot water, filter with fast filter paper, and dilute to 1L. Store in a ground-mouth bottle,bzxz.net
Appendix B
Methods for recovering precious metals
(reference)
B1 Scope of application
This method is applicable to the recovery of precious metals in the filtrate (platinum, butanedione ethanol solution) and (butanedione palladium) after the determination of palladium and the filtrate (sodium bromoplatinate solution) after the oxidation and hydrolysis of sodium bromate when determining the main elements. B2 Principle
The test solution or filtrate containing precious metals and the solution after treatment and dissolution of precipitate, when the pH value is 3-4, use hydrated hydrazine to reduce the precious metal compound to sponge-like gold lips, B3 Reagents and solutions
B3.1 Hydrochloric acid (GB622):
B3.2 Nitric acid (GB626);
B3.3 Hydrazine hydrate (HGB3200)
B3.4 Sodium bicarbonate (GB640) solution: 100g/L, B4 Operation steps
B4.1. Recovery of precious metals in the remaining test solution
Transfer the excess test solution in the volumetric flask into a 500mL beaker, heat to 60℃, add hydrated hydrazine (B3.4) dropwise while stirring until the precipitation is complete, heat to boiling, make the precipitate condense, and the solution becomes clear. Filter with slow quantitative filter paper while hot, and wash the precipitate with water until there is no chloride ion.
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Transfer the precipitate into the weighed medium, dry and ashed, place the medium with precipitate in a high temperature furnace, burn at 800℃ for 1h, take out, cool and weigh.
B4.2 Recovery of precious metals in platinum, diacetyl alcohol solution and diacetyl palladium precipitate Transfer the platinum and diacetyl alcohol solution into a 500mL beaker, heat and evaporate until nearly dry, put in diacetyl palladium precipitate, add 30mL aqua regia (hydrochloric acid (B3.1)-nitric acid (B3.2) = 3+1) to dissolve, heat and evaporate to about 10mL, then add hydrochloric acid (B3.1) three times, 10mL each time, evaporate to nearly dry, add about 80mL water, heat and boil, adjust to pH 3~4 with sodium bicarbonate solution (B3.3), and cool the solution to about 60℃. The following operations are the same as those specified in B4.1. B4.3 Recovery of precious metals in sodium bromoplatinate solution Transfer the sodium bromoplatinate solution to a 500mL beaker, heat and evaporate to about 10mL, then add hydrochloric acid (B3.i) three times, 10mL each time, and evaporate to nearly,
Add about 80mL of water, heat to boiling, adjust the pH value to 3-4 with sodium bicarbonate solution (B3.3), and cool the solution to about 60℃. The following operations are the same as those specified in B4.1, with additional instructions:
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China; this standard is under the jurisdiction of the fertilizer catalyst standardization technical unit of the Ministry of Chemical Industry; this standard was drafted by Taiyuan Fertilizer Plant; the main drafters of this standard are Pan Yu'e, Nie Lihua, Chen Youming, Han Jinjing, Wang Shuping, 12
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A1.1 Cobalt (II) nitrate;
A1.2 Ammonium nitrate (GB659);
A1.3 Ammonia water (GB631);
A1.4 Activated carbon (powder):
A1.5 Nitric acid (GB626);
HG/T 2271.2—92
Preparation of hexaammine cobalt (II) nitrate and its saturated solution (supplement)
A2 Preparation of hexaammine cobalt (III) nitrate Dissolve 73 of cobalt (II) nitrate (A1.1) in 100mL of water, add 80g of ammonium nitrate (A1.2), 2g of activated carbon (A1.4) and 100mL of ammonia water (A1.3). After air is passed through the solution for 3-4 hours, 1300-1500 mL of water acidified with 50 mL of nitric acid (A1.5) is added and heated on a water bath until the yellow precipitate is dissolved. Then the solution is filtered to remove the activated carbon. 200 mL of nitric acid is added to the filtrate and an orange crystalline precipitate is precipitated after cooling. It is filtered with a quartz sand core funnel, washed with mother liquor and ethanol, and dried in an oven at 100°C. It is stored in a ground-mouth bottle for later use. A3 Preparation of saturated solution of hexaammine cobalt nitrate (II) Weigh 17 g of hexaammine cobalt nitrate (II) prepared in Chapter A2, dissolve in 200 mL of hot water, filter with fast filter paper, and dilute to 1 L. Stored in a ground-mouth bottle,
Appendix B
Method for recovering precious metals
(reference)
B1 Scope of application
This method is applicable to the recovery of precious metals in the remaining test solution after the determination of the main elements, the filtrate (platinum, butanedione ethanol solution) and (butanedione palladium) when determining palladium and the filtrate (sodium bromoplatinate solution) after the oxidation and hydrolysis of sodium bromate when determining butane. B2 Principle
The test solution or filtrate containing precious metals and the solution after treatment and dissolution of precipitate, when the pH value is 3-4, use hydrated hydrazine to reduce the precious metal compound to sponge-like gold lips, B3 Reagents and solutions
B3.1 Hydrochloric acid (GB622):
B3.2 Nitric acid (GB626);
B3.3 Hydrazine hydrate (HGB3200)
B3.4 Sodium bicarbonate (GB640) solution: 100g/L, B4 Operation steps
B4.1. Recovery of precious metals in the remaining test solution
Transfer the excess test solution in the volumetric flask into a 500mL beaker, heat to 60℃, add hydrated hydrazine (B3.4) dropwise while stirring until the precipitation is complete, heat to boiling, make the precipitate condense, and the solution becomes clear. Filter with slow quantitative filter paper while hot, and wash the precipitate with water until there is no chloride ion.
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Transfer the precipitate into the weighed medium, dry and ashed, place the medium with precipitate in a high temperature furnace, burn at 800℃ for 1h, take out, cool and weigh.
B4.2 Recovery of precious metals in platinum, diacetyl alcohol solution and diacetyl palladium precipitate Transfer the platinum and diacetyl alcohol solution into a 500mL beaker, heat and evaporate until nearly dry, put in diacetyl palladium precipitate, add 30mL aqua regia (hydrochloric acid (B3.1)-nitric acid (B3.2) = 3+1) to dissolve, heat and evaporate to about 10mL, then add hydrochloric acid (B3.1) three times, 10mL each time, evaporate to nearly dry, add about 80mL water, heat and boil, adjust to pH 3~4 with sodium bicarbonate solution (B3.3), and cool the solution to about 60℃. The following operations are the same as those specified in B4.1. B4.3 Recovery of precious metals in sodium bromoplatinate solution Transfer the sodium bromoplatinate solution to a 500mL beaker, heat and evaporate to about 10mL, then add hydrochloric acid (B3.i) three times, 10mL each time, and evaporate to nearly,
Add about 80mL of water, heat to boiling, adjust the pH value to 3-4 with sodium bicarbonate solution (B3.3), and cool the solution to about 60℃. The following operations are the same as those specified in B4.1, with additional instructions:
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China; this standard is under the jurisdiction of the fertilizer catalyst standardization technical unit of the Ministry of Chemical Industry; this standard was drafted by Taiyuan Fertilizer Plant; the main drafters of this standard are Pan Yu'e, Nie Lihua, Chen Youming, Han Jinjing, Wang Shuping, 12
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Standard Express Network m.bzioia.com Free download of various American standard industry materials AL reagent
A1.1 Cobalt (II) nitrate;
A1.2 Ammonium nitrate (GB659);
A1.3 Ammonia water (GB631);
A1.4 Activated carbon (powder):
A1.5 Nitric acid (GB626);
HG/T 2271.2—92
Preparation of hexaammine cobalt (II) nitrate and its saturated solution (supplement)
A2 Preparation of hexaammine cobalt (III) nitrate Dissolve 73 of cobalt (II) nitrate (A1.1) in 100mL of water, add 80g of ammonium nitrate (A1.2), 2g of activated carbon (A1.4) and 100mL of ammonia water (A1.3). After air is passed through the solution for 3-4 hours, 1300-1500 mL of water acidified with 50 mL of nitric acid (A1.5) is added and heated on a water bath until the yellow precipitate is dissolved. Then the solution is filtered to remove the activated carbon. 200 mL of nitric acid is added to the filtrate and an orange crystalline precipitate is precipitated after cooling. It is filtered with a quartz sand core funnel, washed with mother liquor and ethanol, and dried in an oven at 100°C. It is stored in a ground-mouth bottle for later use. A3 Preparation of saturated solution of hexaammine cobalt nitrate (II) Weigh 17 g of hexaammine cobalt nitrate (II) prepared in Chapter A2, dissolve in 200 mL of hot water, filter with fast filter paper, and dilute to 1 L. Stored in a ground-mouth bottle,
Appendix B
Method for recovering precious metals
(reference)
B1 Scope of application
This method is applicable to the recovery of precious metals in the remaining test solution after the determination of the main elements, the filtrate (platinum, butanedione ethanol solution) and (butanedione palladium) when determining palladium and the filtrate (sodium bromoplatinate solution) after the oxidation and hydrolysis of sodium bromate when determining butane. B2 Principle
The test solution or filtrate containing precious metals and the solution after treatment and dissolution of precipitate, when the pH value is 3-4, use hydrated hydrazine to reduce the precious metal compound to sponge-like gold lips, B3 Reagents and solutions
B3.1 Hydrochloric acid (GB622):
B3.2 Nitric acid (GB626);
B3.3 Hydrazine hydrate (HGB3200)
B3.4 Sodium bicarbonate (GB640) solution: 100g/L, B4 Operation steps
B4.1. Recovery of precious metals in the remaining test solution
Transfer the excess test solution in the volumetric flask into a 500mL beaker, heat to 60℃, add hydrated hydrazine (B3.4) dropwise while stirring until the precipitation is complete, heat to boiling, make the precipitate condense, and the solution becomes clear. Filter with slow quantitative filter paper while hot, and wash the precipitate with water until there is no chloride ion.
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Transfer the precipitate into the weighed medium, dry and ashed, place the medium with precipitate in a high temperature furnace, burn at 800℃ for 1h, take out, cool and weigh.
B4.2 Recovery of precious metals in platinum, diacetyl alcohol solution and diacetyl palladium precipitate Transfer the platinum and diacetyl alcohol solution into a 500mL beaker, heat and evaporate until nearly dry, put in diacetyl palladium precipitate, add 30mL aqua regia (hydrochloric acid (B3.1)-nitric acid (B3.2) = 3+1) to dissolve, heat and evaporate to about 10mL, then add hydrochloric acid (B3.1) three times, 10mL each time, evaporate to nearly dry, add about 80mL water, heat and boil, adjust to pH 3~4 with sodium bicarbonate solution (B3.3), and cool the solution to about 60℃. The following operations are the same as those specified in B4.1. B4.3 Recovery of precious metals in sodium bromoplatinate solution Transfer the sodium bromoplatinate solution to a 500mL beaker, heat and evaporate to about 10mL, then add hydrochloric acid (B3.i) three times, 10mL each time, and evaporate to nearly,
Add about 80mL of water, heat to boiling, adjust the pH value to 3-4 with sodium bicarbonate solution (B3.3), and cool the solution to about 60℃. The following operations are the same as those specified in B4.1, with additional instructions:
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China; this standard is under the jurisdiction of the fertilizer catalyst standardization technical unit of the Ministry of Chemical Industry; this standard was drafted by Taiyuan Fertilizer Plant; the main drafters of this standard are Pan Yu'e, Nie Lihua, Chen Youming, Han Jinjing, Wang Shuping, 12
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