Methods of test for stabilized soils, Part 9: Determination of the bituminous stabilizer content of bitumen and tar-stabilized soils

IS 4332 Part 9 (1970) - Introduction & Key Specifications

• Scope: Method to determine bituminous stabilizer content in bitumen/tar stabilized soils.
• Applicability: Not suitable above ambient temperature 30°C due to solvent evaporation.
• Material Quantity: As per Table 1 (Clause 12.1) - quantities for test samples.
• Duplicate Test Reporting (Clause 14.3):
  • If difference > 0.4 (units), discard & repeat test.
  • If ≤ 0.4, report individual and mean values.
• Apparatus (Clause 10.1):
  • Hot extractor with:
    • Cylindrical brass gauze container (3 mm mesh), diameter 125-200 mm.
    • Brass/welded iron pot with cover, gasket, swiveling bolts.
    • Graduated receiver (10 ml) & reflux condenser.
    • Heater (electric/gas).
    • Filter paper.
• Rounding off results: As per IS 2-1960.

Apparatus Dimensions Summary

graph LR
A[Soil Sample] --> B[Hot Extractor]
B --> C[Solvent Extraction]
C --> D[Condensation & Collection]
D --> E[Measurement in Receiver]
E --> F[Calculate Bituminous Content]

This standard ensures reliable quantification of bitumen/tar content for stabilized soil quality control.

IS 4332 Part 9: Scope - Key Specifications & Tables

Scope Summary:

• This part specifies the method to determine the bituminous stabilizer content (bitumen and tar) in stabilized soils.
• Applicable for soils stabilized with bituminous materials under ambient temperatures ≤ 30°C.
• Not suitable for climates exceeding 30°C due to solvent evaporation.

Key Table: Sample Size for Determination (Clause 12.1, Table 1)

Reporting Criteria (Clause 14.3)

• Duplicate test results differing by > 0.4 are discarded; test repeated.
• If difference ≤ 0.4, report individual values and mean.

Procedure Highlights (Clause 13.1)

• Dry filter paper at 100–120°C, cool in desiccator, weigh.
• Sample warmed slightly, representative portion weighed per Table 1.
• Sample placed in gauze-lined cylinder, solvent added, extraction performed with reflux condenser ensuring steady reflux (2-5 drops/sec).

This method ensures accurate quantification of bituminous stabilizer content for quality control in soil stabilization projects.

flowchart TD
  A[Soil Sample] --> B[Quartering & Weighing (Table 1)]
  B --> C[Place in Filter Paper-lined Cylinder]
  C --> D[Add Solvent (800-1500 ml)]
  D --> E[Fix Reflux Condenser]
  E --> F[Heat & Extract (2-5 drops/sec)]
  F --> G[Collect Extract & Analyze]
  G --> H{Duplicate Test Results}
  H

IS 4332 Part 9: Grouping of Soil

Soil Grouping (Clause 2.1)

Soils are classified based on particle size passing specific IS sieves:

Sample Preparation Weights (Clause 5.1, Table 5)

Stabilizer Content Formula (Clause 7.2)

[ S_2 = \frac{\text{Weight of bituminous stabilizer}}{\text{Weight of dry soil}} \times 100% ]

Where:

• (a) = weight of water in the sample (from IS 4332 Part 2)
• (W_g) = weight of the sample

Summary

• Grouping by sieve size helps identify soil type for stabilization.
• Sample weights vary by soil type for testing accuracy.
• The stabilizer content is calculated as a percentage of dry soil weight.

flowchart TD
    A[Soil Sample] --> B{Particle Size}
    B -->|>90% < 2.36 mm| C[Fine-Grained Soil]
    B -->|>90% < 20 mm| D[Medium-Grained Soil]
    B -->|>90% < 40 mm| E[Coarse-Grained Soil]
    C --> F[Sample Weight 150-200 g]
    D --> G[Sample Weight 1000-1500 g]
    E --> H[Sample Weight 5000-6000 g]

This classification and sample preparation ensure standardized testing of stabilized soils per IS 4332 Part 9.

IS 4332 Part 9 - Apparatus Specifications Summary

1. Hot Extractor (Clause 10.1)

• Cylindrical Container (Fig. 4)

  • Material: Brass gauze, ~3 mm thickness
  • Diameter (A): 125 mm to 200 mm (as needed)
  • Diameter (B): 125 mm to 250 mm (as needed)
  • Features: 6-8 equally spaced slots for swiveling bolts; rests on 3 pegs or a stool inside pot.

• Outer Pot (Fig. 5)

  • Material: Brass or welded iron
  • Diameter (A): 125 mm to 225 mm
  • Diameter (B): 200 mm to 375 mm
  • Flanged with cover & asbestos gasket; cover secured by swiveling bolts with wing nuts.

• Assembled Apparatus (Fig. 6)

  • Includes brass gauze cylinder inside pot with cover.
  • Internal jet diameter: 15.2 mm

• Graduated Receiver (Fig. 7)

  • Capacity: 10 ml
  • Connected for reflux condensation with adequate cold water flow.

• Heater

  • Electric plate or gas ring recommended.

• Filter Paper

  • Suitable for filtration after extraction.

2. Additional Apparatus (Clauses 3.7 - 3.10)

• Graduated Measuring Cylinders: 1000 ml, 500 ml, 250 ml.
• Filter Candle: Porous alumina/porcelain, ~80 mm length, 30 mm diameter, pore size 2-4 μm.
• Burette: 50 ml with two-way tap (Fig. 2).
• Recovery Apparatus: Water bath (~15 cm diameter), manometer, vacuum reservoir, vacuum source (Fig. 3).

Key Dimensions Summary Table

IS 4332 Part 9 - Reagents and Apparatus Key Points

Reagents (Clause 4.1)

• Dichloromethane (Methylene chloride): Minimum 95% purity, boiling range 39 - 40.5°C.
• Silica Gel: Powdered, must pass through a 75-micron IS sieve.

Apparatus Specifications

Notes:

• Filter assembly uses a metal or cork ring, connected to air pressure source (Fig. 1 & 2).
• Hot extractor must have sufficient cold water flow for solvent condensation.
• Heater can be electric or gas ring.

flowchart LR
    A[Sample] --> B[Hot Extractor (Brass gauze container)]
    B --> C[Solvent Extraction with Dichloromethane]
    C --> D[Condensation in Receiver (10 ml)]
    D --> E[Filtration through Porous Alumina Filter Candle]
    E --> F[Measurement via Burette]

This setup ensures precise bituminous stabilizer content determination in stabilized soils per IS 4332 Part 9.

IS 4332 Part 9 - Preparation of Sample: Key Points

1. Reagents Quality (Clause 4.1)

• Dichloromethane (Methylene chloride): 95% purity, boiling range 39–40.5°C.
• Silica gel: Powdered, passing 75-micron IS sieve.
• Solvent: Pure toluene as per IS 536-1968.

2. Sample Preparation (Clause 5.1)

• Break bulk sample into small pieces (slight warming allowed).
• Successive quartering to obtain representative sample weight.

3. Sample Size Based on Grading (Clause 12.1)

4. Procedure Highlights (Clause 13.1)

• Dry filter paper at 100–120°C, cool in desiccator, weigh accurately.
• Place filter paper inside gauze cylinder lining.
• Weigh sample into lined cylinder (±0.05% accuracy).
• Place cylinder inside extractor pot; add 800–1500 ml solvent.
• Bolt cover with dried gasket; add water to receiver to graduation.
• Heat to maintain steady reflux (2–5 drops/sec).

IS 4332 Part 9: Test Procedure Key Points

Sample Size (Table 1 - Clause 12.1)

Procedure Highlights (Clause 13.1)

• Dry filter paper at 100-120°C, cool in desiccator, weigh.
• Line gauze cylinder with filter paper.
• Weigh sample accurately (nearest 0.05%).
• Place sample in cylinder, add 800-1500 ml solvent.
• Assemble reflux condenser; maintain steady reflux of 2-5 drops/sec.
• For large samples, perform extraction in two operations.

Reporting Results (Clause 14.3)

• If duplicate test results differ by >0.4%, discard and retest.
• If difference ≤0.4%, report individual and mean values.
• Express stabilizer content to nearest 0.1% (Clause 8.2).

flowchart TD
    A[Sample Preparation] --> B[Dry & Weigh Filter Paper]
    B --> C[Line Gauze Cylinder]
    C --> D[Weigh Soil Sample]
    D --> E[Place Sample in Cylinder]
    E --> F[Add Solvent & Assemble]
    F --> G[Heat & Reflux 2-5 drops/sec]
    G --> H[Extract & Collect Data]
    H --> I{Duplicate Test?}
    I -->|Yes| J[Check Difference ≤ 0.4%]
    J -->|Yes| K[Report Mean & Individual Values]
    J -->|No| L[Discard & Repeat Test]

This procedure ensures accurate determination of bituminous stabilizer content in soils as per IS 4332 Part 9.

IS 4332 Part 9 - Key Calculations & Specifications

1. Reporting of Results (Clause 14.3)

• If difference between duplicate test results > 0.4, discard and repeat test.
• If difference ≤ 0.4, report individual values and their mean.

2. Material Quantities (Clause 12.1)

• Use quantities as per Table 1 (not provided here).

3. Drying to Constant Weight (Clause 13.4)

• Dry washed aggregate at 100-120°C until weight difference < 0.05% over successive half-hour intervals.
• Cool in desiccator before weighing.

4. Insoluble Portion of Stabilizer (Clause 6.5)

• Determine insoluble matter by dissolving stabilizer in dichloromethane.
• Filter through Gooch/sintered silica crucible or filter paper.
• Calculate % soluble stabilizer ( P ) by:

[ P = \frac{\text{Weight of soluble stabilizer}}{\text{Total weight of stabilizer}} \times 100 ]

Summary Table for Reporting Duplicate Tests

For detailed insoluble matter determination, refer IS:1215-1978.

flowchart TD
    A[Start Test] --> B[Perform Duplicate Determinations]
    B --> C{Difference ≤ 0.4?}
    C -- Yes --> D[Report Values & Mean]
    C -- No --> E[Discard & Repeat Test]

This ensures accuracy and reliability in stabilizer content and aggregate testing.

IS 4332 Part 9 - Reporting of Results (Clause 14.3)

• When performing duplicate determinations, if the difference between the two results exceeds 0.4, both results must be discarded and the test repeated.
• If the difference is ≤ 0.4, report both individual values and the mean value.

Summary Table for Reporting:

Reporting format example:

This ensures accuracy and reliability in test reporting as per IS 4332 Part 9.

If you need formulas for related calculations (e.g., stabilizer content), refer to Clause 7.2:

[ S_2 = \frac{\text{weight of stabilizer}}{\text{weight of dry soil}} \times 100 ]

Let me know if you want details on that!

IS 4332 Part 9: Test Conditions for Ambient Temperature > 30℃

Context:
IS 4332 (Part IX) covers determination of bituminous stabilizer content in stabilized soils. Section B specifically addresses test modifications when ambient temperature exceeds 30℃ due to high solvent evaporation rates affecting accuracy.

Key Specifications & Procedures for Ambient Temperature > 30℃

• Problem: High evaporation rate of solvent at >30℃ affects test accuracy.
• Modification: Use reduced pressure (vacuum) during solvent evaporation to control frothing and evaporation.

Vacuum Pressure Control (Clause 6.2)

• Vacuum can be created by water filter-pump or mechanical vacuum pump.
• This controlled vacuum minimizes frothing and solvent loss.

Reporting Results (Clause 14.3)

• Results expressed as % stabilizer to nearest 0.1%.
• Duplicate tests must not differ by more than 0.4%; otherwise, repeat test.
• Report individual and mean values if difference ≤ 0.4%.

Summary Table: Test Conditions for Ambient Temperature > 30℃

flowchart TD
    A[Start Test] -->

Hot Extractor Apparatus Details (IS 4332 Part 9)

Apparatus Components (Clause 10.1):

• Cylindrical Container (Fig. 4):

  • Made of brass gauze (~3 mm mesh)
  • Diameter (A): 125–200 mm
  • Height (B): 125–250 mm
  • Supported inside a brass or welded iron pot (Fig. 5) by three pegs or a stool.

• Pot (Fig. 5):

  • Brass or welded iron, flanged with cover and asbestos gasket ring
  • Diameter (A): 125–225 mm
  • Height (B): 200–375 mm
  • Cover fixed with swiveling bolts and wing nuts.

• Receiver (Fig. 7):

  • Graduated 10 ml receiver for solvent condensation
  • Adequate reflux container with cold water flow.

• Heater:

  • Electric plate or gas ring to maintain steady reflux (2–5 drops/sec).

• Filter Paper:

  • Dried at 100–120°C, cooled in desiccator, weighed, and fitted inside the gauze cylinder (Clause 13.1).

Sample Size Table (Clause 12.1)

Operating Conditions:

• Solvent Volume: 800–1500 ml depending on extractor size.
• Heating: Adjust to avoid local overheating; maintain steady reflux.
• Pressure Control (Clause 6.2):
  • For bitumen emulsions/tars >42°C equiviscous temp: reduce pressure to 150 mm Hg during frothing stage.
  • For petroleum oils

IS 4332 (Part 9) - Solvent Specifications Summary

1. Solvent Purity (Clause 11.1)

• Solvent: Pure toluole as per IS: 536-1968 (Industrial Toluole specification).

2. Sample Size (Clause 12.1 & Table 1)

• Sample warmed slightly, quartered for representative portion.
• Sample placed in gauze-lined filter paper inside extractor.

3. Extraction Procedure (Clause 13.1)

• Filter paper dried at 100-120°C, cooled in desiccator, weighed.
• Solvent volume: 800-1500 ml depending on extractor size.
• Heat applied to maintain reflux of 2 to 5 drops/sec.
• Water added to receiver for volume correction.

4. Insoluble Portion (Clause 6.5)

• Use dichloromethane (95% purity) for solubility tests.
• Insoluble matter filtered through Gooch/sintered silica crucible or filter paper.
• Calculate soluble stabilizer percentage (P).
• Refer IS: 1215-1978 for insoluble matter determination.

5. Reagents Quality (Clause 4.1)

• Analytical reagent grade.
• Dichloromethane boiling range: 39–40.5°C.
• Silica gel: powdered, passing 75-micron IS sieve.

flowchart TD
    A[Sample Collection] --> B[Dry Filter Paper (100-120°C)]
    B --> C[Weigh Filter Paper]
    C --> D[Place Sample in Gauze-lined Filter Paper]
    D --> E[Add Solvent

IS 4332 Part 9 - Sample Size Requirements

Key Specifications (Clause 5.1 & 12.1)

Samples shall be reduced by hand and quartered to obtain representative weights as per soil type:

Additional Notes:

• Slight warming may be used to facilitate sample reduction.
• Clause 12.1 confirms quantities must follow Table 1 (weights as above).
• Solvent purity for tests: Pure toluene as per IS 536-1968 (Clause 11.1).
• Reporting (Clause 14.3): If duplicate test results differ by >0.4, discard and repeat.

Summary Table for Sample Preparation

| Soil Type          | Sample Weight (g) |
|--------------------|-------------------|
| Fine-grained       | 150 - 200         |
| Medium-grained     | 1,000 - 1,500     |
| Coarse-grained     | 5,000 - 6,000     |

This ensures representative, standardized sampling for reliable testing per IS 4332 Part 9.

IS 4332 Part 9: Extraction Procedure - Key Points

Apparatus (Clause 10.1)

• Hot extractor with:
  • Brass gauze cylindrical container (3 mm mesh), diameter 125-200 mm.
  • Brass or welded iron pot, diameter 125-375 mm.
  • Cover with asbestos gasket and swiveling bolts.
  • Graduated receiver (10 ml), reflux condenser.
  • Heater (electric/gas).
  • Suitable filter paper (dried at 100-120℃).

Sample Size (Table 1, Clause 12.1)

Procedure (Clause 13.1 & 13.2)

• Dry filter paper at 100-120℃, weigh, fit inside gauze cylinder.
• Warm sample slightly, quarter to required weight.
• Place sample on filter paper inside gauze cylinder.
• Pour 800-1500 ml solvent (size-dependent) over sample.
• Bolt cover with gasket, add water to receiver to mark.
• Heat pot to maintain steady reflux: 2-5 drops/sec.
• Water collects in receiver; solvent refluxes over sample, extracting soluble matter.

Reagents (Clause 4.1)

• Dichloromethane (95%, boiling 39-40.5℃).
• Powdered silica gel (passes 75-micron sieve).

flowchart TD
    A[Prepare Sample] --> B[Dry & Weigh Filter Paper]
    B --> C[Place Sample in Filter Paper inside Gauze Cylinder]
    C --> D[Place Cylinder in Pot]
    D --> E[Add Solvent (800-1500 ml)]
    E --> F[Bolt Cover with Gasket

IS 4332 Part 9: Calculation and Reporting (Clause 14.3)

Key Specification for Reporting Results:

• When performing duplicate determinations, if the difference between the two results exceeds 0.4, both results must be discarded and the test repeated.
• If the difference is ≤ 0.4, report:
  • Both individual values
  • The mean value

Summary Table for Reporting Criteria

Formula for Mean Value

[ \text{Mean} = \frac{X_1 + X_2}{2} ]

Where:

• (X_1, X_2) = results of duplicate determinations

Additional Notes:

• Ensure all measurements are taken after drying samples to constant weight (difference <0.05% between weighings).
• Follow sample quantity requirements as per Table 1 (Clause 12.1).
• Stabilizer content formula and other calculations are detailed in earlier clauses (e.g., Clause 7.2).

flowchart TD
    A[Start Duplicate Tests] --> B{Difference > 0.4?}
    B -- Yes --> C[Discard Results & Repeat Test]
    B -- No --> D[Report Individual Values]
    D --> E[Calculate & Report Mean]
    E --> F[End]

This ensures accuracy and reliability in test reporting per IS 4332 Part 9.