SH/T 0341-1992 Determination of alumina content in catalyst carriers

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Card type: Test method

1. Method number / full title / English name / replacement relationship

• Standard number: SH/T 0341-92
• Chinese title: Determination of alumina content in catalyst carriers
• English title: not provided in the available source
• Replacement relationship: replaces SY 2771-78S
• Year confirmation information: the source marks “(20(14 year confirmation)”, suspected to be “(2014 year confirmation)”, requires confirmation against the source standard (source-text extraction)
• Approval/implementation: approved by China Petrochemical Corporation 1992-05-20, implemented on 1992-05-20

2. Scope of application and non-applicability

• Scope of application: This standard specifies the method for determining alumina content in catalyst carriers; it is applicable to catalyst carriers with alumina as the matrix.
• Non-applicability: not provided in the available source.

3. Method principle

The sample is dissolved with sulfuric acid, hydrochloric acid and hydrogen peroxide. The aluminum in the solution complexes with disodium ethylenediaminetetraacetate (EDTA). The excess EDTA is back-titrated with zinc chloride standard titration solution using xylenol orange as indicator, with hexamethylenetetramine as buffer and pH as 5～6, and the alumina content is calculated from the consumed volume.

4. Reagents and materials (purity / preparation)

• 4.1 Hydrochloric acid: analytical grade, prepared as 1:1 (by volume ratio) solution.
• 4.2 Ammonia water: analytical grade, prepared as 1:? (by volume ratio) solution. The source text is “prepared as l: (by volume ratio) solution”, the ratio number requires confirmation against the source standard (source-text extraction).
• 4.3 Hexamethylenetetramine: analytical grade.
• 4.4 Zinc chloride: analytical grade.
• 4.5 Xylenol orange indicator.
• 4.6 Disodium ethylenediaminetetraacetate (EDTA): analytical grade.
• 4.7 Sulfuric acid: analytical grade.
• 4.8 30% Hydrogen peroxide: analytical grade.
• 4.9 Sodium chloride: analytical grade.
• 4.10 Potassium nitrate: analytical grade.
• 4.11 Zinc oxide: primary standard reagent.
• 4.12 Eriochrome black T indicator.
• 4.13 Water: deionized water, conductivity not greater than 5 μs/cm. The source text is “5ps/cmo”, the unit requires confirmation against the source standard (source-text extraction).
• 4.14 Ammonium chloride: analytical grade. The source text is “ammonium chloride”, requires confirmation against the source standard (source-text extraction).

5.1 Preparation of xylenol orange indicator

Weigh 1 g xylenol orange and 100 g sodium chloride, mix and grind finely, then place in a ground-glass stoppered bottle.

5.2 Preparation of Eriochrome black T indicator

Weigh 1 g Eriochrome black T and 100 g sodium chloride, mix and grind finely, then store in a ground-glass stoppered bottle. The source text is “Eriochrome black T”, requires confirmation against the source standard (source-text extraction).

5.3 c(EDTA)=0.05 mol/L (0.05M) Preparation and standardization of disodium ethylenediaminetetraacetate standard titration solution

• 5.3.1 Preparation: Weigh 19 g EDTA, dissolve in water, transfer to a 1 L volumetric flask, dilute to the mark, and mix well. This standard titration solution should be standardized once every half month.
• 5.3.2 Standardization: Weigh 0.13 g primary standard zinc oxide that has been ignited at 800℃ to constant mass, to the nearest 0.0002 g. Moisten with a small amount of water, add 2 mL hydrochloric acid solution (clause 4.1) to dissolve it, then add 10 mL water. Neutralize with ammonia water solution (clause 4.2) to pH 7～8. Then add 10 mL ammonia-ammonium chloride buffer solution (pH=10) and about 0.1 g Eriochrome black T indicator, and titrate with the prepared EDTA solution until the solution changes from purple to pure blue. Carry out a blank test simultaneously.
  • Note: The preparation of ammonia-ammonium chloride buffer solution (pH=10) is to weigh 54.0 g ammonium chloride, dissolve in water, then add 350 mL ammonia water, and dilute with water to 1 L. The source text is “350.L”, requires confirmation against the source standard (source-text extraction).
• 5.3.3 Calculation: The actual concentration of the EDTA standard titration solution c(EDTA), mol/L, is calculated according to formula (1):
  • The formula area in the source text source-text extraction is severely incomplete, the complete expression of formula (1) requires confirmation against the source standard (source-text extraction). Visible elements: M (mass of zinc oxide, g), V₁ (volume of EDTA solution used, mL), V₀ (volume of EDTA solution used in the blank test, mL), 0.08138 (mass of zinc oxide in grams equivalent to 1.00 mL EDTA standard titration solution [c(EDTA)=1.000 mol/L]).
  • In the source formula, “mass of M— zinc chloride, g” contradicts the primary standard zinc oxide used for standardization, suspected to be “zinc oxide”, requires confirmation against the source standard (source-text extraction).

5.4 c(ZnCl₂)=0.05 mol/L Preparation of zinc chloride standard titration solution

Weigh 6.9 g zinc chloride, add a small amount of water to dissolve; to accelerate dissolution, add dropwise a small amount of hydrochloric acid to dissolve it completely, then dilute to 1 L.

5.5 Volume ratio of EDTA standard titration solution to zinc chloride standard titration solution

Take 25 mL EDTA standard titration solution and place in a 250 mL conical flask, add about 100 mL water, then add 0.1 g xylenol orange indicator, 1.5 g hexamethylenetetramine, and titrate with zinc chloride standard titration solution until a wine-red color appears as the endpoint. The volume ratio of the two solutions K is calculated according to formula (2). The source formula (2) source-text extraction is incomplete, the complete expression requires confirmation against the source standard (source-text extraction).

5. Instruments and equipment

• 3.1 Beaker: 250, 500 mL
• 3.2 Volumetric flask: 1000 mL
• 3.3 Measuring cup: 25 mL
• 3.4 Pipette: 50 mL
• 3.5 Burette: 50 mL
• 3.6 Wash bottle: 500 mL
• 3.7 Funnel: diameter 60 mm
• 3.8 Conical flask: 250 mL
• 3.9 Dropping bottle
• 3.10 High-temperature furnace

6. Recommended operating conditions

• Dissolution: sulfuric acid 15 mL, heat on electric furnace until sulfuric acid just fumes white; add 20 mL hydrochloric acid solution, 2 mL 30% hydrogen peroxide; heat gently until sulfuric acid just fumes white.
• Complexation and back-titration pH: 5～6 (hexamethylenetetramine buffer).
• Indicator: xylenol orange.
• Titration endpoint: solution changes from yellow to wine-red.
• Ignition residue determination: 850℃ constant temperature 1 h.
• Other recommended operating conditions: not provided in the available source.

7. Sampling and sample preparation

• 6.1 Sample treatment: Weigh a sample ground to about 150 mesh, 0.5 g (to the nearest 0.0002 g), into a 250 mL beaker, rinse the beaker walls with a small amount of water, add sulfuric acid 15 mL, cover with a watch glass, heat on an electric furnace until sulfuric acid just fumes white, remove and cool. Add 20 mL hydrochloric acid solution, 2 mL 30% hydrogen peroxide, and when bubbling stops, place again on the electric furnace and heat gently until sulfuric acid just fumes white, remove the beaker and cool, wash the watch glass and beaker walls with water until the solution volume in the beaker is 50 mL. Place on the electric furnace and boil, then cool, transfer the solution to a 100 mL volumetric flask, dilute to the mark, and mix well. If the boiled solution has suspended matter, it must be filtered and washed with hot water.
• 6.3.1 Ignition residue sample: While weighing the sample in clause 6.1, weigh 0.5～1 g (to the nearest 0.0002 g) of sample into a constant-mass covered porcelain crucible, place in a high-temperature furnace, raise the temperature to 850℃, hold at constant temperature for 1 h, then remove, place in a desiccator to cool to room temperature (about 0.5 h), and weigh.

8. Analysis procedure

• 6.2 Use a pipette to take 10 mL from the sample solution of clause 6.1 into a 250 mL conical flask, accurately add 25.00 mL EDTA standard titration solution, 50 mL water and 0.? g xylenol orange indicator (the indicator mass is illegible in the source transcription and remains unverified), adjust to wine-red with ammonium hydroxide (clause 4.2) solution, then adjust with hydrochloric acid solution (clause 4.1) until it just turns yellow, then add 1 more drops, heat and boil for 1 min. Remove and cool, add 1～2 g hexamethylenetetramine so that the pH value is 5～6. Titrate with zinc chloride standard titration solution until the solution changes from yellow to wine-red.
• 6.3 Determination of ignition residue: see 6.3.1 (section 7) and 6.3.2 calculation.

9. Qualitative and quantitative determination and calculation formulas

6.3.2 Ignition residue B[%(m/m)] calculated according to formula (3)

B = (m₂ − m₀) / m₁ × 100 …… (3)

• m₀: mass of the crucible after constant mass, g
• m₁: mass of the sample before ignition, g
• m₂: total mass of the sample and crucible after ignition, g
• Take the arithmetic mean of the results of repeated tests as the ignition residue.

7 Calculation: alumina content in the sample X[%(m/m)] calculated according to formula (4)

X = [(V₂ − V₃·K) × c(EDTA) × F × 0.05098] / (m · B) × 100 …… (4) When K=1: X = [(V₂ − V₃) × c(EDTA) × F × 0.05098] / (m · B) × 100

• V₂: the volume of EDTA standard titration solution added, mL
• V₃: the volume of zinc chloride standard titration solution consumed during titration, mL
• c(EDTA): the actual concentration of the EDTA standard titration solution, mol/L
• F: the dilution factor of the test sample
• K: the volume ratio of the EDTA standard titration solution to the zinc chloride standard titration solution
• m: the mass of the test sample, g
• B: ignited basis, %(m/m)
• 0.05098: the mass of aluminum oxide, expressed in grams, equivalent to 1.00 mL EDTA standard titration solution [c(EDTA)=1.000 mol/L]
• Note: In the original formula (4), the symbol V₂ is source-text extraction as “inkstone”, and V₃ is “Yao”; they have been restored according to context and require confirmation against the source standard (source-text extraction).

10. Precision

Repeatability: the difference between two results of repeated determinations by the same operator shall not be greater than 2% of their arithmetic mean.

11. Report

Take the arithmetic mean of two results of repeated determinations as the determination result.

12. Normative References

not provided in the available source (the main text does not list a normative reference document list).

13. Source and verification

This page is an AI translation of the available Chinese method card. Human verification is pending. It is not an official translation of the standard. Check the source standard and product certificate before use.

14. Quick Q&A Reference