SH/T 0508-1992 Determination of Oil Content in Oil Shale (Low-Temperature Retorting 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.

Source limitations: The source heating schedule is incomplete and its time-temperature correspondence is unresolved. The negative heating-tolerance wording, extracted sample quantities, equation numbering and semicoke precision column require confirmation. The missing equation is not reconstructed. Values below reproduce the source card and are not independently validated.

Card type: test method

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

• Standard number: SH/T 0508-92
• Full title: Determination of Oil Content in Oil Shale (Low-Temperature Retorting Method)
• English title: not provided in the available source.
• Replacement relationship: replaces ZBh 22001-86 (the source reads "replaces ZBh. 22001- 86"; requires confirmation against the source standard).
• Approval/implementation: approved by China Petrochemical Corporation on 1992-05-20 and implemented on 1992-05-20.

2. Scope and exclusions

• This standard specifies a method for determining the oil content of a test sample by low-temperature retorting.
• This standard applies to determining the oil yield and by-product yields from low-temperature retorting of oil shale.
• Exclusions: not provided in the available source.

3. Principle

Place the test sample in an aluminum retort. With air excluded, heat at a specified rate to 520℃ and hold for a specified time. After retorting, determine the yields of oil, water, semicoke and retorting by-products.

4. Reagents and materials (purity / preparation)

• 4.1 Petroleum jelly: technical grade.
• 4.2 Emery: grade 800.
• Appendix A: A2.1 Toluene (analytical grade) or industrial solvent naphtha.
• Appendix B: B2.2 The desiccator contains indicating silica gel or lumps of anhydrous calcium chloride as desiccant.

5. Apparatus

• 5.1 Aluminum retort: see Figure 1; effective volume 170 mL ± 10 mL.
• 5.2 Crusher: adjustable particle size, for sample preparation.
• 5.3 Heating furnace: single-hole or multi-hole electric furnace rated at 2 kW, including a pyrometer and thermocouple (the source reads "thermocouple (FA)"; requires confirmation against the source standard).
• 5.4 Receiver: 250 mL conical flask.
• 5.5 Weighing bottle: diameter 60 mm.
• 5.6 Standard sieve: square openings of 3 mm.
• 5.7 Analytical balance: sensitivity 0.1 mg.
• Appendix A: A3.1 Water determination apparatus (see Figure A1): includes receiver 4 (conical flask), capacity 250 mL; water measuring tube 3 (as in GB/T 260), and straight condenser 2, length 250~300 mm. A3.2 Automatically temperature-controlled electric heating mantle: capacity 250 mL.
• Appendix B: B2.1 Drying oven (with automatic temperature control and an internal blower, capable of maintaining 105~110℃); B2.2 desiccator; B2.3 glass weighing bottle (diameter 40 mm, height 25 mm, with ground-glass lid) or porcelain dish (outer diameter 40 mm, height 16.5 mm, wall thickness 1.5 mm, with close-fitting lid); B2.4 analytical balance (accurate to 0.0002 g).

6. Recommended operating conditions

• Strictly control the heating rate according to Table 1. During heating, the measured temperature at each time interval shall not exceed the specified value by -5℃ (the source reads "-59C"; requires confirmation against the source standard; the direction of this tolerance is unresolved).
• On reaching 520℃, hold for 20 min, then stop heating.
• Table 1, aluminum retort heating schedule (the extracted table is severely incomplete; only some values are legible): heating times 0, 10, 20, 30, 40, 50 min and temperatures 185, 300, 410, 475, 520℃. The time-temperature correspondence requires confirmation against the source standard because the table is incomplete.
• Appendix A: adjust the distillation rate so that 2~4 drops fall per second from the lower end of the condenser.
• Appendix B: oven temperature 105~110℃; dry for 1 h with forced airflow.

7. Sampling and sample preparation

• 6.3 Crush the sample to a particle size below 3 mm, take a representative 50 g portion into an iron tray, dry under laboratory conditions for 24 h, then transfer to a wide-mouth bottle with a ground-glass stopper for later use. (The source reads "5009", suspected to mean 50 g; requires confirmation against the source standard.)
• 6.4 Thoroughly mix the prepared sample using a horn spoon. Place 50 g ± 0.5 g in a weighing bottle of known mass, weigh to 0.01 g, and transfer the sample of known mass into the aluminum retort. Keep sample out of the outlet tube and make its surface as level as possible. (The source fragments "509[unclear sign]0.59" and "0.019" require confirmation against the source standard.)
• Appendix B: weigh 1 g ± 0.1 g of the analysis sample with particle size below 0.2 mm (accurate to 0.0002 g).

8. Analysis procedure

• 6.1 Check the aluminum retort for gas tightness.
  • 6.1.1 Checking procedure: apply soapy water to all joints of the closed retort, or immerse the retort body 10~15 mm below the water surface. Introduce gas until the retort pressure reaches 1471~1961 Pa (150~200 mmH₂O), and maintain it for about 1 min. No bubbles indicates satisfactory gas tightness. If the outlet tube leaks, tighten the connecting nut further or remove the outlet tube for inspection. If the retort body-to-lid joint leaks, lap it as described in 6.1.2.
  • 6.1.2 Lapping procedure: coat the mating surfaces of the retort body and lid with a mixture of petroleum jelly and grade 800 emery. Insert a metal rod 7~8 cm long into the small hole in the lid. Hold the rod with one hand and the retort body with the other; rotate back and forth through 90° several times, then turn through 180°. Do not apply pressure to the lid while lapping. Once the body and lid fit tightly, wipe off the emery/petroleum jelly mixture with a soft cloth, wash with water and dry. Repeat the gas-tightness test until satisfactory.
• 6.2 Before using a new aluminum retort, heat it to 530℃, hold for 20 min, then cool, remove and set aside.
• 6.4 Transfer the sample of known mass into the aluminum retort.
• 6.5 Fit the retort lid and gently tap it tight with a wooden mallet. Connect the retort outlet tube to the receiver of known mass using a rubber stopper. The outlet tube shall extend into the receiver by at least half the receiver height without touching its bottom. Insert a slightly bent glass tube through the other small stopper hole and connect it to the gas collection apparatus (see Figure 2). All connections must be gas-tight.
• 6.6 Put ice and water in the cooling bath and immerse the receiver in the water, keeping its mouth slightly above the water surface.
• 6.7 Switch on the electric heating and strictly control the heating rate according to Table 1. On reaching 520℃, hold for 20 min, then stop heating.
• 6.8 Open the furnace lid, remove the thermocouple and immediately remove the aluminum retort and receiver. Disconnect the receiver from the rubber-stopper joint at the retort outlet. Plug the outlet tube with a cork to prevent the semicoke from absorbing moisture from the air.
• 6.9 Wipe water from the receiver exterior, leave for about 5 min, then weigh to 0.01 g. The difference between the mass of the receiver containing condensate and the empty receiver is the mass of retorting condensate (oil plus water).
• 6.10 Determine water in the condensate by solvent extraction. Subtract the water mass from the condensate mass to obtain the shale oil mass.
• 6.11 Once the aluminum retort has cooled to room temperature, gently tap the rear handle of its body with a wooden mallet until the lid loosens. Remove the lid, pour the semicoke into a weighing bottle of known mass and weigh immediately. Brush all semicoke adhering to the retort wall into the bottle. Subtract the bottle mass from the measured mass to obtain the oil-shale semicoke mass.
• 6.12 Determine moisture in the analysis sample by the moisture determination method in GB 212.
• 6.13 Determine water in the condensate according to Appendix A.
• Appendix A:
  • A4.1 Add 100 mL of toluene or industrial solvent naphtha to the previously weighed receiver containing retorting condensate.
  • A4.2 Connect the receiver tightly to its matching dry, calibrated water measuring tube with a ground-glass joint. Connect the top of the measuring tube to a dry condenser.
  • A4.3 Loosely plug the upper end of the condenser with cotton or other material to keep out dust and prevent atmospheric moisture from condensing inside it.
  • A4.4 Apply electric heat and control the distillation rate so that 2~4 drops fall per second from the lower end of the condenser. Stop distillation when the water in the measuring tube no longer increases and the solvent becomes completely clear. Near the end, increase the distillation rate to carry all droplets adhering to the condenser wall into the water measuring tube.
  • A4.5 After the receiver cools, dismantle the apparatus. If water remains on the measuring-tube wall, move a spiral wire up and down and allow it to stand for several minutes. Read the water volume after the droplets have fully settled (for calculation, the density of water at room temperature may be taken as 1).
• Appendix B:
  • B3 Using a previously dried and weighed weighing bottle (or porcelain dish), weighed to 0.0002 g, weigh 1 g ± 0.1 g of analysis sample with particle size below 0.2 mm (accurate to 0.0002 g). Remove the lid and place the bottle (or dish) in an oven already operating with forced airflow at 105~110℃. Dry the sample for 1 h with continuous airflow, remove the bottle (or dish) and replace the lid. Cool in air for 2~3 min, then in a desiccator to room temperature (about 20 min), and weigh.
  • Carry out further check-drying periods of 30 min each until the mass change is below 0.001 g or the mass increases. In the latter case, use the mass measured immediately before the increase for calculation. Retain the porcelain dish and sample for ash determination. Check drying is not performed when moisture is below 2%.

9. Identification, quantification and calculations

• 7.1 Calculate retorting-product yields on the analysis basis using the following equations:

  Tf = (a - b) / m × 100 ……(1)

  T = Tf × 100 / (100 - Wf) ……(2)

  Wf = Wc + Wz ……(3) (the correspondence between equation numbers and symbols requires confirmation against the source standard).

  Kf = c / m × 100 ……(5) (the source numbering jumps to (5); (4) is not present in the available source).

  Where:

  • Tf — shale oil yield on the analysis basis, % (m/m);
  • T — shale oil yield on the dry basis, % (m/m);
  • m — mass of the analysis sample, g;
  • a — mass of condensate, g;
  • b — total water mass from retorting, g;
  • Wf — total retorting water yield on the analysis basis, % (m/m);
  • Wc — moisture content of the analysis sample, % (m/m);
  • Wz — pyrolysis water yield on the analysis basis, % (m/m);
  • Kf — oil-shale semicoke yield on the analysis basis, % (m/m);
  • c — mass of oil-shale semicoke, g.

• 7.2 Report sample oil content as a mass percentage. Take the arithmetic mean of duplicate determinations and round to one decimal place.

• Appendix A: A5 Calculate the total retorting water mass percentage Wf using equation (A1):

  Wf = V / m × 100 ……(A1)

  Where: V — water volume in the receiver condensate, mL; m — sample mass, g. Report sample water content as a mass percentage to one decimal place.

• Appendix B: B4 Calculate the result using equation (B1):

  W = M1 / m × 100 ……(B1)

  Where: W — moisture of the analysis sample, %; M1 — mass lost by the analysis sample after drying; m — mass of the analysis sample, g. Report moisture of the analysis sample as a mass percentage.

10. Precision

Judge the reliability of test results according to the following provisions (95% confidence level).

• 8.1 Repeatability: in the same laboratory, the difference between duplicate results obtained by the same operator shall not exceed the values in Table 2:

  Table 2, % (m/m)

  Sample oil content	Oil content	Water	Semicoke
  < 10	0.4	0.4	1.0
  10~20	0.8	0.4	1.0
  > 20	1.5	0.4	1.0

• 8.2 Reproducibility: the difference between results obtained by different operators in different laboratories shall not exceed the values in Table 3:

  Table 3, % (m/m)

  Sample oil content	Oil content	Water	Semicoke
  < 10	0.8	0.8	1.5
  10~20	1.2	0.8	1.5
  > 20	2.0	0.8	1.5

  (The extracted semicoke column of Table 3 reads "15 [unreadable character]5 1.5"; requires confirmation against the source standard. The source card arranges it as 1.5 by reference to the correspondence in Table 2; this remains unverified.)

11. Report

• 7.2 Report sample oil content as a mass percentage. Take the arithmetic mean of duplicate determinations and round to one decimal place.
• Appendix A: report sample water content as a mass percentage to one decimal place.
• Appendix B: report moisture of the analysis sample as a mass percentage.

12. References

• GB 212, Proximate Analysis of Coal (source-card editor's note: current designation GB/T 212, title Proximate Analysis of Coal; current status has not been independently verified here).
• GB/T 260 (referenced for the water measuring tube in Appendix A; source wording: "as in GB/T 260").

13. Source and verification

• Additional information: technical administration and drafting by Fushun Research Institute of Petroleum and Petrochemicals. Main drafters: Chen Jiying and Liu Changshan.

14. Quick-reference questions