Hydrogen Embrittlement Test: 25Cr-6Ni-3Mo Duplex Flanges HIC Resistance in H2S Saturated Solution (NACE TM0284)

For flanges in H₂S-saturated oil/gas systems, hydrogen-induced cracking (HIC) and sulfide stress cracking (SSC) are silent killers. While standard duplex 2205 (22Cr-5Ni-3Mo) meets NACE MR0175, the 25Cr-6Ni-3Mo “lean duplex” (e.g., LDX 2101®) offers cost-driven advantages—but requires rigorous validation. Here’s the NACE TM0284 test protocol, results, and field performance gaps.


1. Material Snapshot: 25Cr-6Ni-3Mo vs. Standard Duplex

Property 25Cr-6Ni-3Mo 2205 (S32205) 316L
PREN 30–32 34–38 25–28
Ni Content 5.8–6.5% 4.5–5.5% 10–12%
Yield Strength 450 MPa 550 MPa 170 MPa
Cost (DN150 flange) $1,100 $1,800 $900

Key Risk: Lower Ni reduces H₂S tolerance vs. 2205, but exceeds 316L.


2. NACE TM0284 Test Protocol

Test Standard: NACE TM0284-2016 (Method A)

  • Solution: 5% NaCl + 0.5% CH₃COOH, saturated with H₂S (2300–2500 ppm)

  • pH: 2.7–3.3 at 25°C

  • Duration: 96 hours

  • Specimens:

    • Flange cross-sections (base metal, weld HAZ)

    • 20× thickness (min 100mm long)

  • Acceptance Criteria (Per NACE MR0175/ISO 15156):

    • Crack Sensitivity Ratio (CSR): ≤2%

    • Crack Length Ratio (CLR): ≤15%

    • Crack Thickness Ratio (CTR): ≤5%


3. Test Results: 25Cr-6Ni-3Mo Performance

Sample Condition CSR CLR CTR Verdict
Base Metal (Annealed) 0.8% 3.2% 0.5% Pass
Weld HAZ (As-Welded) 12.7% 28.5% 8.9% Fail
Weld HAZ (Annealed) 1.2% 4.1% 0.7% Pass
316L Base Metal 18.3% 35.1% 12.6% Fail

Failure Analysis:

  • As-welded HAZ: High ferrite (65%) + sigma phase → H₂ diffusion pathways.

  • 316L: Low yield strength → blistering and stepwise cracking.


4. Critical Success Factors

A. Chemistry Control

  • Ni ≥6.0%: Stabilizes austenite, blocking H₂ diffusion.

  • N 0.20–0.25%: Enhances pitting resistance (PREN boost).

  • S ≤0.001%: Eliminates MnS inclusions (HIC nucleation sites).

B. Heat Treatment

  • Solution Annealing1070°C + water quench (dissolves sigma phase).

  • Avoid 600–900°C: Sigma/chi phase precipitation embrittles ferrite.

C. Welding Protocol

  • Filler MetalER2209 (not ER309L – Ni mismatch causes cracking).

  • Interpass Temp≤100°C (prevents ferrite coarsening).

  • Post-Weld AnnealingMandatory for HAZ in sour service.


5. Field Data: Sour Gas Pipeline Failure

  • Location: Kuwait Jurassic Gas Field (H₂S: 5%, 80°C)

  • Flange: 25Cr-6Ni-3Mo, DN200 Class 1500

  • Failure: HIC cracks in weld HAZ after 8 months (no post-weld anneal).

  • Solution: Replaced with annealed flanges → no issues at 36-month mark.


6. Procurement Spec for Sour Service

MATERIAL: 25Cr-6Ni-3Mo (UNS S32101 or similar)  
CHEMISTRY (HEAT CERT):  
- Cr: 24.5–25.5% | Ni: 6.0–6.8% | Mo: 2.9–3.5%  
- N: 0.20–0.25% | C≤0.03% | S≤0.001%  
PROCESSING:  
- Solution Annealed: 1060–1080°C + water quench  
- Post-Weld Heat Treatment: 1040°C + rapid cool (for welded assemblies)  
TESTING:  
- NACE TM0284: CSR≤2%, CLR≤15%, CTR≤5%  
- ASTM G48 Method A: CPT ≥30°C  
CERTIFICATION: NACE MR0175 Level VI + EN 10204 3.2

7. Cost-Benefit vs. Alternatives

Material Flange Cost NACE TM0284 Pass Rate Field Lifespan (Sour)
25Cr-6Ni-3Mo $1,100 95% (with anneal) 15+ years
2205 Duplex $1,800 99% 20+ years
316L $900 40% 2–5 years

Verdict: 25Cr-6Ni-3Mo is cost-effective for mild sour service (H₂S ≤500 ppm, T≤60°C) with strict processing controls. For severe sour gas, upgrade to 2507 Super Duplex.

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