Original standard number ZB G75005-88 HG/T 3543-1988 Chemical composition analysis method of natural gas reforming catalyst HG/T3543-1988 Standard download decompression password: www.bzxz.net

Professional Standard of the People's Republic of China
ZB G.75005:88
Conversion H/1 43 -88
Analytical method of chemical composition for natural gas reforming catalysts198·8-04-14 Issued
Issued by the Ministry of Chemical Industry of the People's Republic of China and implemented on December 1, 1988
Professional Standard of the People's Republic of China
Analytical 'method oft chemical compositionltfon tornatural gas reforming catalysts1Subject content and scope of application
ZBG75005—88
This standard specifies the chemical analysis methods for natural gas reforming catalysts models Z107, Z108, 7.201 and Z205 and other products with similar chemical compositions.
Mubiaotui is applicable to the determination of aluminum oxide, nickel oxide, silicon dioxide, iron oxide, calcium oxide, potassium oxide and sodium oxide content in natural gas reforming catalyst.
2 Reference Standards
HG1--150083Z102 Natural Gas--stage Reforming Catalyst HG 11546
Chemical Composition Analysis Method of Light Oil Steam Reforming Catalyst84
ZB G 75001: 86
ZB G 75002-- 86
Analysis Method of Trace Sulfur in Fertilizer Catalyst
Analysis Method of Trace Chlorine in Fertilizer Catalyst
ZB G 75003—86
Analysis Method of Loss on Ignition of Fertilizer Catalyst
ZB G 75004-- 86
Method for analyzing moisture in fertilizer catalysts
3 Preparation of samples for analysis
Mix the samples evenly and take about 20g of the sample by quartering. Crush and grind it in a porcelain mortar until it passes through a 0.125mm sieve. Divide it into two parts, keep one for future reference, and put the other into a weighing bottle. Bake it in an oven at 105-110℃ for 1h. Take it out and cool it in a dryer for chemical component analysis.
4 Melting of samples
4.1 Summary of methods
Add a mixed flux of sodium carbonate and boric acid to the sample and melt it at high temperature. Leach the melt with dilute hydrochloric acid and take the liquid for the determination of aluminum, nickel, iron, silicon and calcium.
4.2 Reagents
All reagents used are analytically pure unless otherwise specified. 4.2.1 Sodium carbonate (GB639-77);
4.2.2 Boric acid (GB628-78);
4.2.3 Mixed flux: anhydrous sodium carbonate and boric acid 2:3, mix and grind evenly 4.2.4 Sweet acid (GB62277): I+1 solution. 4.3 Instruments
4.3. Laboratory - General instruments and volume is 30~50 ml. Platinum (with cover). 4.4 Operation steps
Approved by the Ministry of Chemical Industry of the People's Republic of China on April 11, 1988, and implemented on 1988-12-01
.ZB G 75005-88
Weigh 0.5 g of the dried sample (accurate to 0.0002 wt%) and place it in a platinum crucible. Weigh 5 g of the mixed flux (4.2.3) (leave a little for covering) and pour it into a platinum crucible. Stir with a platinum wire, cover with a layer of mixed flux, and then put it in a high-temperature furnace. Heat at 200°C (hold for 10 min. Then heat to 950°C to melt for 2 min. h.
Take out the platinum, cool it and place it in a 250mL beaker, add 25mL of hydrochloric acid (4.2.4) and 75mL of water, and heat to extract. After the melt is completely dissolved, cool it to room temperature, transfer it to a 250mL volumetric flask, dilute it to the scale with water, shake it well, and use it for the determination of aluminum oxide, nickel oxide, silicon oxide, iron oxide and calcium oxide.
5 Determination of aluminum oxide content
5.1 Method summary
Add the EDTA standard solution to the solution with a pH of 3 to 5, so that aluminum, nickel, iron and titanium ions are all mixed with EDTA. TA forms a complex, the remaining EDTA solution is back-titrated with a standard zinc fluoride solution, and then sodium fluoride is added to displace the EDTA complexed with aluminum and titanium, and titrated with a standard zinc nitride solution to measure the total content of aluminum and titanium. 5.2 Reagents
All reagents used are analytically pure unless otherwise specified. 5.2.1 Ammonia (GB631-77): 1+1;
5.2.2 Sodium fluoride (GB1264-77)
5.2.3 Methyl orange indicator (HGB308959): 0.05% aqueous solution; 5. 2. 4
Xylenol orange indicator (Q/HG22—1544—75), 0.1% aqueous solution; 5.2.5 Glacial acetic acid (CB67678)
Sodium acetate (GB693---77)
EDTA standard solution: c (EDTA) = 0.02mol/L, preparation method see GB6015.2.7
Zinc standard solution: c (znCl.) = 0.02mol/l. 5.2.8
5.2.9 Acetic acid-sodium acetate buffer solution PH5.5, dissolve 50g acetic acid in appropriate amount of water. Add 2.5mL glacial acetic acid , then dilute to 1000mL with water and shake the spoon.
5.3 Instruments
General laboratory instruments.
5.4 Operating steps
Accurately pipette 10mL of the sample solution prepared in Chapter 4 into a 250mL jar-shaped bottle, add 20mL of EDTA standard solution (5.2.7), one drop of Scintillation orange indicator, adjust with ammonia water (1+-1) until the bath changes from red to yellow, add 10mL of buffer solution (5.2.9), boil for 5min, cool to room temperature with water, add three drops of xylenol orange indicator, and drip with zinc chloride standard solution (5.2.8) until the solution turns from yellow to red. Add about 1 drop of sodium fluoride, boil for another 5min, cool to room temperature with water, and drip with standard zinc chloride solution (5.2.8) until the solution just changes from yellow to red, and record the consumed volume.
5.5 Calculation
The aluminum oxide (Al2O3) content (X2O3) is expressed as mass percentage and is calculated according to formula (1): X ±: V × 0. 050 98 × 100
m × 250
Wherein: m - concentration of zinc chloride standard solution, mol/L: m - amount of zinc fluoride standard solution, mLt
-weight of sample, B1
0.05098 - the mass of aluminum oxide equivalent to 1.00 mL of zinc fluoride solution with cZnCl2) = 1.000 mol/L, g. 5.6 Allowable difference
The difference between two parallel determination results shall not exceed 0.30%. .cOm（1
6 Determination of nickel oxide content
ZBG75005-88
6.1 Method summary
In a weakly acidic solution of pH 5-6, mask the aluminum with sodium fluoride, add a standard solution of EDTA to make the ions completely complexed, use xylenol orange as an indicator, back-titrate the excess EDTA with a standard solution of zinc oxide, and calculate the amount of nickel oxide. 6.2 Reagents
Unless otherwise specified, all reagents used are analytically pure reagents. 6.2. 1 Hydrogen water (GB 6.2.2 Methyl red indicator (HG3-~958-76): 0.1% ethanol solution, weigh 0.1g methyl red and dissolve it in 60mL 95% ethanol, add 10mL water, shake it;
6.2.3 Xylenol orange indicator (Shanghai Q/HG22: 1544--75): 0.1% aqueous solution; 6.2.4 Glacial Z acid (GB 676--- 78);
6.2.5 Sodium acetate (GB693--77)
6.2.6 Acetic acid-sodium acetate buffer solution: pH 5.5. Preparation method see 5.2.9. Zinc oxide standard solution: (ZnCl) = 0.02 mal/L: 6.2.7
B.2: 8 EDTA standard solution: c(EDTA) = 0.02 mol/L: 6.2.9 Sodium fluoride (GB 1264-77).
6.3 Instrumentswww.bzxz.net
General laboratory instruments.
6.4 Operating steps
Accurately pipette 20 mL of the sample solution prepared in Chapter 1 into a 250 mL conical flask, add 20 mL of EDTA standard solution (6.2.8), about 20 mL of water, and one drop of methyl red indicator, and use ammonia water (6.2.1) Adjust the solution until it changes from red to yellow, add 10 mL of acetic acid-sodium acetate buffer (6.2.6) and about 1 mL of sodium fluoride. Slightly boil for 3 min, cool, add 5 mL of buffer solution, and then add two drops of xylenol orange indicator. Add zinc fluoride standard solution (6.2.7) until the solution changes from yellow to red, and record the solution consumption. 6.5 Calculation
Nickel oxide (NiO) content (X.) is expressed as mass percentage and calculated according to formula (2): (/ = s: Vg × 0. 07471 × 100X
Wu Zhong; r
0. 074 71
6.6 Allowable difference
EDTA standard solution concentration, moi/L;
Zinc standard solution concentration, mol/L;
EDTA standard solution added volume, mL;
Zinc standard solution drop volume, mL;
Weigh the sample mass·B;
m×250
Nickel oxide equivalent to 1.00 mL EDTA solution with (EDTA) = 1.000 mol/L: more. The difference between the two parallel determination results shall not exceed 0. 30%. 7 Determination of silicon dioxide content
7.1 Method summary
(2)
Under the conditions of pH 1.5 and certain reagent concentration, temperature and color development time, monosilicic acid and succinate generate β-silicomolybdic acid (also known as silica yellow). Since silica molybdenum yellow is not very stable, it is often reduced to silicomolybdic blue (also known as code blue), which has an absorption peak at around 320nm and is measured at this wavelength. Adding tartaric acid can eliminate the interference of phosphorus and arsenic. 7.2 Reagents
ZB G 7 5 005— 88
Reagents not specifically noted are analytical grade. 7.2.1 Sodium molybdate (HG3-1087-77): 19.5% solution. Weigh 195g of sodium molybdate and dissolve it in a plastic cup filled with hot water (≥60C). After cooling, dilute to 1000mL and store in a plastic bottle. Filter if there is precipitation. 7.2.2 Tartaric acid (GB 129177), 10% solution. Weigh 1.00 tartaric acid and place it in a plastic cup. Dissolve it in water and dilute to 1000mL. mL, stored in a plastic bottle;
7.2.3 Sulfuric acid (HG625-77): c (HSO.) is about 8 mol/L, take 450 mL of sulfuric acid with a density of 1.84 g/mL, add it to 500 mL of water, cool it down and dilute it to 1000 mL with water; 7.2.4: Silica: high purity reagent
7.2.51 Amino-2-phenol-4-sulfonic acid (abbreviated as ANSA or 1.2,4 acid) (HGB333060) 7.2.6 Anhydrous sodium sulfite (HG3-1078-77): 7.2.7
Sodium metabisulfite (HG3-909-76)
7.2.8 Reducing solution: containing ANSA 1.5 mol/L 7.2. 8. 1 Liquid A;
Weigh 7 g of anhydrous sodium sulfite and dissolve it in 50 7.2.8.2 Solution B
Weigh 90 ml of sodium metabisulfite and dissolve it in 900 ml of water: Mix solution A (7.2.8.T) and solution B, dilute to 1000 ml with water, add a pinch, and store in a plastic bottle in a cool place. This solution contains 1.5 g of ANSA per liter.
7.2.9 Anhydrous sodium carbonate (GB 639.-77); 7.2.10 Silicon dioxide standard solution:
7. 2. 10. Silicon dioxide stock solution (containing SiO2, 0.500 mg/mL): Weigh 0.250 g of silicon dioxide (7. 2. 4), place it in a platinum argon solution, add 3 g of anhydrous sodium carbonate, stir well, melt at 950 ℃ for 1 h, take out and cool, put it into a plastic cup and dissolve it with hot water, dilute it to the scale with water in a 500 mL volumetric flask, shake, and immediately transfer it to a plastic bottle for storage. The shelf life of this stock solution is two months: 7.2.10.2 Silicon dioxide standard solution (containing SiO2, 0.010 mg/mL): Pipette 10.00 mL of stock solution (7.2.10.1), transfer to a 600 mL volumetric flask, dilute to scale with water, shake well, and store in a plastic bottle. Prepare this solution when needed; 7.2.11 Hydrochloric acid (GB62277), 1+1 and 1+9 solutions: 7.2.12 Ethanol (GB 676-78):
7.2.13 White monosaccharide blue indicator: 0.1% ethanol solution, weigh 0.05 g of thymol blue and dissolve it in a mixture of 10 mL. ethanol and 40 mL of water, stir well, and filter out any insoluble matter: 7.2.14 Sodium hydroxide (GB629-76): 10% aqueous solution. 7.3 Instruments
7.3.1 General laboratory instruments;
7.3.2 Spectrophotometer.
7.4 Operation steps
7.4.1 Drawing of calibration curve
Accurately pipette 0, 2.00, 4.00, 6.00, 8.00 and 10.00 mL of silica standard solution (7.2.10.2) into six 100 mL volumetric flasks respectively, add water to about 30 mL, add three drops of thymol blue indicator, adjust the solution to a bright red color with hydrochloric acid (1+9), then add 15 mL of hydrochloric acid (19), shake, add 5 mL of sodium lead solution (7.2.1), shake again and let stand for 15 min, add 5 mL of tartaric acid solution (7.2.2) and 11 ml of sulfuric acid (7.2.3), shake, and finally add 2 mL of reducing solution (7.2.8), dilute to the mark with water, and shake. After 10 minutes of standing, use a spectrophotometer at a wavelength of 815nm, with water as the reference and a 2cm absorption cell to measure the absorbance of each standard solution.
Draw a standard curve with the mass of silicon dioxide in the standard solution and the corresponding absorbance value as the horizontal and vertical coordinates respectively. 7.4.2 Determination
ZBG75005—88
Accurately pipette 20ml of the sample solution prepared in Chapter 4 into a 100ml volumetric flask, add three drops of thymol blue indicator, adjust with sodium hydroxide (7.2.14) until the solution changes from red to yellow, then adjust with hydrochloric acid (1+9) until the solution just turns red, add 15ml of hydrochloric acid (1+9), shake well, add 5ml of sodium aluminate solution (7.2.1), shake well and leave for 15min, then add 5ml of tartaric acid (7.2.2), 11ml of sulfuric acid (7.2.3), shake again, and finally add 2ml of reducing solution (7.2.8), dilute to the scale with water, shake well. Leave for 10min, measure the absorbance of the sample solution at the same time as the standard solution under the same conditions as the standard. From the absorbance of the sample solution, find out the mass of silicon dioxide contained from the standard curve. 7.5 Calculation
Silicon dioxide content (X:) is expressed as a mass fraction and calculated according to formula (3): X, = CX10-*
Where: '--Silicon dioxide mass in the sample solution found from the standard curve, m; Weigh the sample mass, 8.
7.6 It is allowed that the difference between the results of two parallel determinations is not less than 0.03%. 8 Determination of ferric trifluoride content
8.1 Method summary
(3)
Use hydroxylamine hydrochloride to reduce trivalent iron ions to monovalent iron ions. At pH 2-9, the monovalent iron ions react with o-phenanthroline to form a red complex, which is determined by spectrophotometry at a wavelength of 510nm. Nickel ions also react with o-phenanthroline to form a colored complex and interfere. Therefore, in the presence of nitriloacetic acid, ammonia water is added to precipitate iron ions and separate them from nickel ions to eliminate the interference of nickel. 8.2 Reagents
All reagents used are analytically pure unless otherwise specified. 8.2.1 Ammonium chloride (0B658-77): 20% solution Ammonia water (GB631-77): 1+1;
8.2.3 Aminoacetic acid (HG3-1110-77); 8.2.4 Electrolyte
Methyl red indicator (HG3-95878): 0.1% solution 8.2.5 Hydrochloric acid (HG622---77) 1+9, 1+99 8.2.6 Hydroxylamine hydrochloride (HG3-967-76): 1% solution 8.2.7 O-phenanthroline (GB1293-77): 0.25% solution, weigh 0.25 B o-phenanthroline, drop it into 50 mL water, add 1 mL concentrated hydrochloric acid, and then dilute with water to 100 mL,
8.2.8 Iron nitride: commercially pure reagent;
8.2.9 Glacial acid (GB 676-78):
8.2.10 Sodium acetate (GB693-77);
8. 2. 11 Acetic acid-sodium acetate buffer solution; pH 4. 9, weigh 54.Dissolve 4g sodium ferric sulfate in 100mL water; add 48mL glacial acetic acid, dilute to 200mL with water, and shake well.
8.2, 12 Ferric fluoride standard solution:
8.2.12.1 Ferric oxide stock solution (containing Fe0, 0.20mg/mL): weigh 0.2008 of ferric oxide (8.2.8) burned and cooled at 600℃, put it into a 100mL beaker, add 10mL of concentrated hydrochloric acid (8.2.5), slowly heat until it is completely dissolved, cool, transfer to a 1000mL volumetric flask, dilute to the scale with water, and shake well; 8.2.12.2 Ferric oxide standard solution (containing Fe0, 0.02m/mL); accurately draw 10mL of stock solution (8.2.12.1), put it into a 100mL volumetric flask; dilute to the scale with water and shake well. 8.3 Instruments
wW. General laboratory instruments and spectrophotometer. 8.4 Operating steps
8.4.1 Drawing of standard curve
ZBG75005-88
Accurately pipette 0, 2.00, 4.00; 6.00, 8.00 and 10.00 mL of ferric oxide standard solution (8.2.12.2): place in six 100 mL volumetric flasks, add water to each until about 50 mL, then add 25 mL of buffer solution (8.2..11), 5 mL of hydroxylamine hydrochloride (8.2.6), and 5 mL of o-phenanthroline solution (8.2.7), dilute with water to the scale, and shake. Let stand for 10 minutes, and measure the absorbance value of each standard solution on the spectrophotometer at a wavelength of 510 nm using a 2 cm absorption cell and water as a reference.
Use the mass of ferric ammine and the corresponding absorbance value as the horizontal and vertical coordinates, respectively, to draw a standard curve. 8.4.2 Determination
Accurately pipette 20mL of the sample solution prepared in Chapter 4 into a 250mL beaker, add water to about 150mL, add 10mL of ammonium chloride (8.2.1), 1 drop of aminoacetic acid and two drops of methyl red indicator, heat the solution to nearly boiling, remove and drop nitrogen water (8.2.2) until the solution changes from red to yellow, filter out the precipitate, wash it three times with water, and the precipitate is used for iron determination. Use 25mL hot (≥60℃) hydrochloric acid (1+9) to dissolve the precipitate in the original beaker. Wash the filter paper three times with hot hydrochloric acid (1+99), about 5mL each time, and add it to the original beaker. After the solution is cooled, add ammonia water (8.2.2) dropwise until a white precipitate appears. Then add hydrochloric acid (1+9) dropwise until the precipitate is just dissolved. Transfer it to a 100mL volumetric flask, add 5mL hydroxylamine hydrochloride solution (8.2.6) and 5mL o-phenanthroline solution (8.2.7), add 25mL buffer (8.2.11), and dilute with water to 4% water. Degree, shake the hook. Leave it for 10 minutes, and measure the absorbance of the test solution with the standard solution under the same conditions, and find the corresponding amount of ferric oxide from the standard curve.
8.5 Calculation
The ferric oxide content (X.) is expressed as a mass fraction, calculated according to formula (4): X,=±×10-1
m×250
Where: m—·The mass of ferric oxide in the test solution found from the standard curve, mB;—． Weigh the mass of the test sample, more. ||tt| |8.6 Allowable error
The difference between the results of two tests shall not exceed 0.03%. 9 Determination of calcium oxide content
9.1 Method summary
Use hexamethylenetetramine and copper reagent to precipitate and separate the interfering ions such as aluminum, iron and iron in the sample solution, and then use triethanolamine to block the remaining aluminum and iron ions.
When the test solution does not contain iron ions, adjust the pH of the above filtrate to 10, use chrome black T as an indicator, and use EDTA standard solution to titrate calcium. Add a small amount of magnesium ethylenetriaminetetraacetate to Make the titration end point change obviously. If the test solution contains magnesium ions, adjust the pH of the filtrate to 12 with potassium hydroxide, use calcium as an indicator, and titrate calcium with EDTA standard solution 9.2 Reagents
Reagent grades not specifically noted are all analytical grade. 9.2.1 Hexamethylenetetramine (GB1400-78): 9.2.2 Steel reagent (HG3-962-76): 2% aqueous solution, prepared when used: 9.2.3
Sodium cyanide (GB1266-77)
9.2. 4 Ethanolamine (Shanghai Q/HG 149-62); 1+[19.2.5
Potassium hydroxide (GB2306-80): 15% aqueous solution; 9.2.6
Eriochrome black T (HGB3086-59): weigh 0.1 chrome black T and 10g sodium fluoride, grind finely, mix; 9. 2.7
ZBG75005-88
Calcium indicator: weigh 0.1B calcium indicator and 10g sodium chloride, grind finely, mix: ammonia water (GB631-77);
Ammonium chloride (GB 658—77):
9.2.10 Ammonia-ammonium chloride buffer solution: pH=10, weigh 27g ammonium oxide (9.2.9) and place it in a beaker, add 325mL water, add 175mL ammonia water after dissolving, and spread evenly;
9.2.11 Disodium ethylenediaminetetraacetic acid (GB1401.78) standard solution: c(EDTA)=0.02mol/L, for the preparation method, see GB6019.2.12 Ethylenediaminetetraacetic acid magnesium solution: c(MgEDTA)=0.005mol/L, for the preparation method, see GB603. 9.3 Instruments
General laboratory instruments.
9.4 Operation steps
Accurately pipette 20mL of the test solution prepared in Chapter 4 into a 250mL beaker, evaporate at low temperature to near T, blow the beaker wall with a small amount of water, add 2g of sodium chloride, stir, add 2g of hexamethylenetetramine and 20mL of copper reagent solution (9.2.2), stir evenly, let stand for 35min, filter, and place the filtrate in a 250mL conical flask. Wash the precipitate with water 56 times, and keep the filtrate for calcium measurement. If the test solution contains magnesium ions, add 4mL of triethanolamine (9.2.4), 15mL of potassium hydroxide (9.2.5) and a small amount of calcium indicator to the above solution, and immediately titrate with EDTA standard solution (9.2.11). The end point is when the solution changes from red to blue. If the test solution does not contain magnesium ions, add 4 mL of ethanolamine (9.2.4), 20 mL of buffer solution (9.2.10), two drops of ethylenediamine (9.2.12) and a little chrome black T indicator, and immediately titrate with EDTA standard solution (9.2.11). The end point is when the solution changes from red to blue.
9. 5 Calculation
Calcium oxide (CaO) content (X,) is expressed as mass percentage and calculated according to formula (5): Xx - -+ × 0.056 08 × 100
Where:
9.6 Allowable difference
m×250
Concentration of EDTA standard solution, mol/L;
Volume of EDTA standard solution titration, mLI
Weigh the mass of the sample, 8!
The mass of calcium oxide equivalent to 1.00 mL EDTA solution with c(EDTA)=1.000 mol/L, bird. When the calcium oxide content is about 10%, the difference between the two parallel determination results is not more than 0.2u. 10 Determination of potassium oxide and sodium oxide content
10.1 Summary of the method
(5)
Most potassium and sodium salts are soluble in water. The potassium and sodium salts in the natural gas conversion catalyst listed in this standard can be leached out with a boiling dilute nitric acid solution. After adjusting the pH, measure it on a flame photometer together with standard potassium and sodium solutions. 10.2 Reagents
All reagents used are analytically pure unless otherwise specified. 10.2.1 Nitric acid (GB626-78): 1% aqueous solution: 10.2.2 Methyl red (HG3-958-76). 0.1% aqueous solution; 10.2.3 Ammonia water (GB631-77): 1+1;
10.2.4 Potassium chloride (GB646-77),
10.2.5 Sodium oxide (GB1266-77)
10.2.6: Mixed standard solution of potassium fluoride and sodium oxide: 10.2.6.1 Potassium oxide standard solution (containing K, 0.100 mg/mL) is weighed and burned at 500~600℃ to a constant amount of potassium chloride 0.7915 g, dissolve in water, dilute to scale with water in a 600.mL volumetric flask, add hook, take out 10 mL from this solution, place in a ZBG75005-88
100mL volumetric flask, dilute to scale with water, shake well; 10.2.6.2 Sodium oxide standard solution (containing Na.00.100m8/mL): weigh 0.9430g of sodium oxide burned to constant weight at 500-600℃, dissolve in water, dilute to scale with water in a 500mL volumetric flask, shake well, take out 10 mL from this solution, place in a 100mL volumetric flask, dilute to scale with water, shake well: 10.2.6.3 Mixed standard solution: Take 5 100mL volumetric flasks, numbered 1 to 5, add insoluble potassium oxide standard solution (10.2.6.1) and sodium oxide standard solution (10.2.6.2) to each flask, then dilute to the mark with water, shake the spoon, and prepare various concentrations of potassium oxide and sodium hydroxide mixed standard solutions. The added volume and the prepared concentration are as follows: mL or g/mL
Standard number
Add standard solution (10.2.6.1) Volume
Potassium oxide standard
μg/mL
Standard solution (10.2.B.2) Volume
Sodium oxide concentration
μg/mL
For example: In standard sample No. 1, add 2mL of potassium oxide standard solution (10.2.6.1) and 4mL of sodium oxide standard solution (10.2.6.2), then dilute with water to 100mL scale and shake well. The concentrations of potassium oxide and sodium oxide in this standard are 2 and 4ug/mL respectively, and the rest are similar.
10.3 Instruments
Laboratory-general instruments and flame photometer.
10.4 Operation steps
10.4.1 Plotting standard working curves of potassium oxide and sodium cyanide. Turn on the instrument according to the flame photometer operation method. Use distilled water to adjust the instrument indications of potassium and sodium to zero. Use No. 5 mixed standard solution (i.e., potassium oxide is 108/mL and sodium oxide is 20ug/mL) to adjust the instrument indications of potassium and sodium to 100 respectively. Then measure the instrument indication values ​​of each mixed standard sample in the middle.
Use the mass of potassium oxide and sodium cyanide in the standard sample as the horizontal axis and the corresponding instrument indication value as the vertical axis to plot the standard working curves of potassium oxide and sodium oxide.
10.4.2 Determination
Weigh 0.5g (accurate to 0.0002g) of the sample prepared in Chapter 3, put it into a 250mL beaker, add 50mL of nitric acid (10).2.1, heat and boil for 20min, add one drop of methyl red indicator, adjust the solution from red to yellow with ammonia water, boil for another 10min, cool, filter into a 100ml volumetric flask, wash the precipitate three times with hot water, add it into a 100mL volumetric flask, dilute to the scale with water, shake well. Determine it together with the standard solution on a flame photometer, and find the corresponding potassium oxide and sodium oxide masses from the standard plot curve according to the instrument indication values ​​of potassium oxide and sodium oxide in the test solution.
10.5 Calculation
Potassium oxide (K,O) content (X,) and sodium oxide (Na,O) content (X,) are expressed as mass percentage and calculated according to formula (6) and formula (7) respectively
R= × 10-
.X 100
WW.bsoso.com(7)
Wu Zhong: k
ZBG75005—88
The amount of potassium oxide in the test solution found from the standard curve is - the amount of sodium oxide in the test solution found from the standard curve, ug, weigh the sample mass, name.
10.6 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.03%. 11
Determination of sulfur content
Determination of chlorine content
Determination according to ZBG75002.
13Determination of loss on ignition
Determination according to ZBC75003.
14Determination of moisture
Determination according to ZB G 75001.
Additional remarks:
This standard is under the jurisdiction of the fertilizer catalyst standardization technical unit of the Ministry of Chemical Industry. This standard was drafted by the Research Institute of Nanjing Chemical Industry Company. The main authors of this standard are Yang Antai and Zhang Xiufang. People's Republic of China
Professional Standard
Chemical Composition Analysis Method of Natural Gas Reforming Catalyst ZB C75005--88
Published by China Standards Press
(Beijing Fuwai Sanlihe)
China Standards Press Printed by Xinhua Bookstore Beijing Distribution Office Distributed by Xinhua Bookstores in various places Sold by the owner without any regulations
Format 880 × 1230 1/16
Qiu Zhang 3/4
February 1989 Edition
"Xueshu 17
199 2!, Printed by Children
Number 1—2 D
1$ 5/: 155066 2-7272
Ting 0.60 pills
Standard date 107—4503%. 11
Determination of sulfur content
Determination of chlorine content
Determination according to ZBG75002.
13Determination of loss on ignition
Determination according to ZBC75003.
14Determination of moisture
Determination according to ZB G 75001.
Additional remarks:
This standard is under the jurisdiction of the fertilizer catalyst standardization technical unit of the Ministry of Chemical Industry. This standard was drafted by the Research Institute of Nanjing Chemical Industry Company. The main authors of this standard are Yang Antai and Zhang Xiufang. People's Republic of China
Professional Standard
Chemical Composition Analysis Method of Natural Gas Reforming Catalyst ZB C75005--88
Published by China Standards Press
(Beijing Fuwai Sanlihe)
China Standards Press Printed by Xinhua Bookstore Beijing Distribution Office Distributed by Xinhua Bookstores in various places Sold by the owner without any regulations
Format 880 × 1230 1/16
Qiu Zhang 3/4
February 1989 Edition
"Xueshu 17
199 2!, Printed by Children
Number 1—2 D
1$ 5/: 155066 2-7272
Ting 0.60 pills
Standard date 107—4503%. 11
Determination of sulfur content
Determination of chlorine content
Determination according to ZBG75002.
13Determination of loss on ignition
Determination according to ZBC75003.
14Determination of moisture
Determination according to ZB G 75001.
Additional remarks:
This standard is under the jurisdiction of the fertilizer catalyst standardization technical unit of the Ministry of Chemical Industry. This standard was drafted by the Research Institute of Nanjing Chemical Industry Company. The main authors of this standard are Yang Antai and Zhang Xiufang. People's Republic of China
Professional Standard
Chemical Composition Analysis Method of Natural Gas Reforming Catalyst ZB C75005--88
Published by China Standards Press
(Beijing Fuwai Sanlihe)
China Standards Press Printed by Xinhua Bookstore Beijing Distribution Office Distributed by Xinhua Bookstores in various places Sold by the owner without any regulations
Format 880 × 1230 1/16
Qiu Zhang 3/4
February 1989 Edition
"Xueshu 17
199 2!, Printed by Children
Number 1—2 D
1$ 5/: 155066 2-7272
Ting 0.60 pills
Standard date 107—45
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