SH/T 0778-2005 Determination of wax content in petroleum asphalt (cracking deoiling method)

AI-translated method card — human verification pending. This is not an official translation of the standard. Unclear source values remain unverified; check the original standard and product certificate before use.

Card type: Test method

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

• Standard number: SH/T 0778—2005
• Chinese name: Determination of wax content in petroleum asphalt (cracking deoiling method)
• English name: Determination of paraffin wax content of asphalts by cracking and deoiling method
• Replacement relationship: This standard is first issued (original text: This standard is first issued)
• Adoption relationship: Modified adoption of DIN EN 12606-1 (confirmed in 2000) "Determination of wax content in petroleum asphalt (cracking yue oil method)" (original text as such, suspected to be "cracking deoiling method", requires confirmation against the source standard (source-text extraction))
• Publication/implementation: published by 2005-11-28, implemented on 2006-06-01
• Issuing authority: National Development and Reform Commission of the People's Republic of China
• Technical administration: Technical administration by Heavy Oil Research Institute of China University of Petroleum (East China)
• Drafting organization: Heavy Oil Research Institute of China University of Petroleum (East China)
• Main drafters: Zhang Yuzhen, Zhang Xiaoying, Chen Jijun

2. Scope of application and non-applicability

• Visible in the original text: "This standard specifies..." "This standard applies to..." "Method for determining wax content in petroleum asphalt by the deoiling method." "Determine the wax content of petroleum asphalt." (source-text extraction severe noise, requires confirmation against the source standard (source-text extraction))
• Explicit applicable object: petroleum asphalt
• Non-applicable scope: not provided in the available source

3. Method principle

Dissolve the distillate oil obtained by cracking distillation with an ether-ethanol mixed solvent, cool and filter at −20 ℃, transfer the precipitated crystals to a bath at 15 ℃, then wash the wax cake with acetone at the same temperature; dissolve the obtained wax with petroleum ether, evaporate the solvent, dry, weigh, and calculate the wax content. (The original text has source-text extraction noise, such as "guoji", "bingmeng", "zhengde wax", "zhengchu rongsu", restored according to context, requires confirmation against the source standard (source-text extraction))

4. Reagents and materials (purity / preparation)

• 4.1 Reagents (listed separately in the original text, specific names missing in many places, requires confirmation against the source standard (source-text extraction))
  • 4.1.1 ...: chemically pure or analytically pure.
  • 4.1.2 ...: chemically pure.
  • 4.1.3 ...: 60 ℃～90 ℃, analytically pure.
  • 4.1.4 ...: chemically pure.
• Reagents confirmed from the main text 5.6, 5.7, 5.9, 5.10: ether, ethanol, ether-ethanol (1:1) mixed solvent, acetone, petroleum ether
• Preparation: ether-ethanol (1:1) mixed liquid (used as washing liquid), pre-cooled to −20.5 ℃±0.5 ℃
• Other purity and preparation details: not provided in the available source

5. Instruments and equipment

• 4.2.1 Two low-temperature cold baths: one cold bath whose temperature can be controlled at −20 ℃±0.2 ℃ (original text ".20Ctu0.2", requires confirmation against the source standard (source-text extraction)); the other cold bath whose temperature can be controlled at 15 ℃±0.5 ℃
• 4.2.2 Glass distillation flask: shape as shown in Figure 1 (cracking flask, unit is millimeters, dimensions marked in the figure include 200, 30, 101, 1～1.5, Ø10±0.5, etc., requires confirmation against the source standard (source-text extraction)); "jiuhangyanbei is the condenser tube" (source-text extraction noise, requires confirmation against the source standard (source-text extraction))
• 4.2.3 Wax freezing filtration apparatus: composed of poly..., glass filter funnel, sample cooling cylinder and column rod stopper, etc., installed as shown in Figure 2; the pore size of the sintered plate in the glass filter funnel is 20 mm～20 μm (original text "20mn-20pm", unit suspected to be incorrect, requires confirmation against the source standard (source-text extraction))
• 4.2.4 Conical flask: 150 mL, equipped with a perforated cork stopper
• 4.2.5 Water jet pump or ...
• 4.2.6 Hot water bath or electric ...
• 4.2.7 Desiccator
• 4.2.8 Gas burner
• 4.2.9 Vacuum drying oven: meets controlled temperature... (specific parameters not provided in the available source)
• 4.2.10 Stopwatch: accurate to 0.1 s (original text "0.18", requires confirmation against the source standard (source-text extraction))
• 4.2.11 Balance: a balance accurate to 0.01 g, 0.001 g (original text "0.00hg", requires confirmation against the source standard (source-text extraction)), 0.0001 g
• Figure 2 Composition of freezing filtration apparatus: 1— rubber support pad; 2— support pad; 3— suction filter bottle; 4— sintered funnel; 5— freezing cylinder; 6— column rod stopper; 7— glass cover; 8— fixed cylinder; 9— cold insulation bath; 10— stopper

6. Recommended operating conditions

• Cracking distillation: directly heated with a gas burner, the flame surrounds the flask; from the start of heating, initial distillation is reached within 5 min～8 min (the first 1 drop flows down from the side arm); continuous distillation at 2 drops per second (4 mL/min～5 mL/min) until distillation ends; the bottom of the flask is heated red within 1 min; distillation from the start of heating to the end is completed within 25 min
• Cooling crystallization: cold bath temperature −20 ℃±0.5 ℃, thermometer immersed to a depth of 150 mm; the coolant liquid level is about 100 mm or more higher than the ether-ethanol liquid level in the sample cooling cylinder; cool for 1 h
• Washing liquid pre-cooling: −20.5 ℃±0.5 ℃
• Natural filtration: 30 min
• Suction filtration speed: about 1 drops per second
• 15 ℃ bath: temperature stable at 30 min
• Vacuum drying: temperature 105 ℃±5 ℃, residual pressure 21 kPa～35 kPa, dry for 1 h; cool in desiccator for 1 h

7. Sampling and sample preparation

• 5.1 Place about 50 g±1 g of sample into the cracking distillation flask (original text "50g1g", requires confirmation against the source standard (source-text extraction)), weighed to the nearest 0.01 g
• 5.3 Heat the distillate oil until melted and carefully shake the receiving bottle to mix the distillate thoroughly; weigh an appropriate amount of sample from it into a 100 mL conical flask of known mass, accurate to 0.001 g, so that the amount of wax obtained after cooling and filtration is between 50 mg～100 mg; the sampling amount of distillate oil shall not exceed 10 g
• Difference from DIN EN 12606-1: DIN specifies a sampling amount of 25 g, this standard specifies a sampling amount of 50 g; DIN takes 1 test points from each cracked oil to make two parallel data, this standard increases sampling from cracked oil to three test points

8. Analysis steps

• 5.1 Load about 50 g±1 g of sample, weighed to the nearest 0.01 g, cover the distillation flask tightly with a cork stopper; use a 150 mL conical flask of known mass as the receiver, immersed in a beaker containing crushed ice; a small groove is cut on the side of the receiver cork to allow non-condensable gas to escape; directly heat with a gas burner
• 5.2 Adjust the flame intensity, reach initial distillation within 5 min～8 min; continuously distill at 2 drops per second (4 mL/min～5 mL/min) until distillation ends; heat the bottom of the flask red within 1 min; complete the whole process within 25 min; after distillation ends, residual distillate oil in the side arm shall not flow into the receiver; weigh the distillate oil to the nearest 0.01 g
• 5.3 Melt and mix the distillate oil, weigh an appropriate amount of sample (accurate to 0.001 g), so that the wax amount is between 50 mg～100 mg, sampling amount not exceeding 10 g
• 5.4 Turn on the cold bath switch, set the refrigeration temperature so that the cold bath temperature remains at −20 ℃±0.5 ℃, thermometer immersed to a depth of 150 mm
• 5.5 Assemble the suction filter bottle, glass filter funnel, sample cooling cylinder and column rod stopper as shown in Figure 2
• 5.6 Add 10 mL of ether to the 100 mL conical flask containing the distillate oil, dissolve thoroughly, then transfer to the sample cooling cylinder; rinse the conical flask twice with 15 mL of ether and pour into the sample cooling cylinder; then add 25 mL of ethanol for mixing
• 5.7 Place the cooling filtration apparatus into the cold bath that has reached the pre-cooling temperature, cool for 1 h to allow sufficient crystallization; place 30 mL 1:1 of ether and ethanol mixed liquid (used as washing liquid) in a test tube with a ground stopper, place in the cold bath and cool to −20.5 ℃±0.5 ℃
• 5.8 Remove the column rod stopper, filter the slurry; hang the column rod stopper in the sample cooling cylinder; maintain natural filtration for 30 min
• 5.9 Start the suction filtration device, maintain the filtrate filtration speed at about 1 drops per second; when the filtrate on the wax layer is about to be exhausted, add at one time 30 mL of ether-ethanol (1:1) mixed solvent pre-cooled to −20.5 ℃±0.5 ℃, wash the wax layer, column rod stopper and inner wall of the sample cooling cylinder, and continue filtering
• 5.10 When the cold wash liquid is no longer visible on the wax layer, remove the cooling filtration apparatus from the cold bath and transfer it to a bath at a temperature of 15 ℃±0.5 ℃; after the temperature has stabilized for 30 min, wash the crystalline wax with 30 mL acetone that was previously placed in the 15 ℃±0.5 ℃ bath, then filter with suction using a vacuum pump; when the cold wash liquid is no longer visible on the wax layer, continue suction filtration for 5 min to suction the solvent in the wax dry
• 5.11 Remove the cooling filtration apparatus from the bath, take off the suction flask, and replace it with a recovery flask of known mass; after reaching room temperature, use petroleum ether heated to 30 ℃～40 ℃ with 100 mL to dissolve the wax on the glass filter funnel, sample cooling cylinder, and plunger
• 5.12 Place the wax recovery flask on a suitable heat source and distill to remove the petroleum ether, then place it in a vacuum drying oven and dry for 1 h; vacuum drying oven temperature 105 ℃±5 ℃, residual pressure 21 kPa～35 kPa; then place the wax recovery flask in a desiccator to cool for 1 h, and weigh to the nearest 0.0001 g

9. Qualitative and Quantitative and Calculation Formulas

• Carry out the cracking distillation operation once according to clauses 5.1 and 5.2, and carry out the dewaxing operation three times according to clauses 5.3～5.12
• The wax content in asphalt X (%) is calculated according to the following formula: X = 100%·(D·P)/(S·d) Where:
  • S—— sample sampling amount, g
  • D—— distillate oil amount, g
  • d—— sample taken from the distillate oil, g
  • P—— mass of wax obtained, g
• Report processing (Chapter 8): On graph paper or a computer, take the obtained wax mass (g) as the abscissa and the wax mass fraction as the ordinate, determine the relationship line, and use interpolation to determine the wax mass fraction when the wax mass is 0.075 g as the reported wax content (%)
• Note: The direction coefficient of the relationship line is taken as positive only; when there are two lines, take the interpolated value
• Difference from DIN EN 12606-1: Considering the relationship between solvent dosage and wax content, the processing of test results in this standard adopts the linear interpolation method

10. Precision

It is considered correct when the difference between each other does not exceed the following values:

• Difference from DIN EN 12606-1: This standard determines the value ranges of repeatability and reproducibility according to the range of wax content, improving precision

11. Report

• See Chapter 8: On graph paper or a computer, take the obtained wax mass (g) as the abscissa and the wax mass fraction as the ordinate to determine the relationship line, and use interpolation to determine the wax mass fraction when the wax mass is 0.075 g as the reported wax content (%)
• Note: The direction coefficient of the relationship line is taken as positive only; when there are two lines, take the interpolated value

12. Normative References

• Chapter 2 Normative references: GB/T 614 "Technical Conditions for Liquid Thermometers for Petroleum Product Testing" (original text "CB /T614", requires confirmation against the source standard (source-text extraction))
• The remaining content of Chapter 2 of the original text source-text extraction has severe noise ("the following attack items", "the amendment sheet/not", "whether it can be used", etc.), requires confirmation against the source standard (source-text extraction)
• Differences stated in the foreword: Delete the referenced standards in the original standard and replace them with the corresponding standards of our country

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 Reference for Questions and Answers