Sample-to-FCL Qualification Process

Switching TiO2 suppliers or qualifying a new grade requires structured validation. Skipping steps risks quality problems at production scale that are difficult to diagnose. The standard 4-stage qualification process minimizes risk and provides a documented trail if quality issues surface later.

Stage 1: Sample request and CoA review

Stage 1: Sample request and CoA review (Week 1)

Sample size: typically 5–25 kg, sometimes up to 100 kg for free.

What we send: - Sample TiO2 in original 25 kg paper bag (or smaller sealed container) - Full batch CoA - SDS - Technical data sheet (TDS) - Recommended dispersion procedure

Buyer activities: - Review CoA against specification target - Verify regulatory compliance (REACH letter, FDA, food contact as needed) - Compare TiO2 content, tinting strength, color, heavy metals against current reference - Decision: proceed to lab batch or reject

Time: 5–10 working days for sample arrival; review takes 1–3 days.

Stage 2: Laboratory batch trial

Stage 2: Laboratory batch trial (Week 2–3)

Lab batch size: typically 100–1000 g of finished product.

Standard test sequence for paint: 1. Disperse TiO2 in formulation per standard procedure 2. Measure Hegman dispersion grade 3. Make drawdown on contrast card 4. Measure contrast ratio (ISO 6504-3) 5. Measure CIE L*a*b* on the drawdown 6. Compare gloss at 60° if relevant 7. Run accelerated weathering (QUV-A 100 hr minimum) if outdoor 8. Compare results against current reference TiO2

Standard test sequence for plastic masterbatch: 1. Compound 50% MB on small twin-screw extruder 2. Extrude 50 μm test film at 50% loading 3. Count fish-eye defects per 100 cm² 4. Measure Δb* before and after 280°C / 5 min 5. Compare against current reference

Standard test sequence for ink: 1. Mill TiO2 in test ink vehicle for 60 min 2. Measure Hegman 3. Drawdown print test 4. Compare opacity, gloss, anilox release against reference

Acceptance criteria: - Critical parameters within ±5% of reference (or tighter for premium applications) - No catastrophic failures (e.g., film defects, color anomalies) - Cost-performance analysis vs incumbent

Time: 1–2 weeks lab work + analysis.

Stage 3 and 4: Pilot production and first FCL

Stage 3: Pilot production batch (Week 4–6)

Pilot batch size: typically 100–500 kg of finished product (1–5 t of TiO2).

Process: - Order sample quantity sufficient for 1 production batch - Receive within 2–4 weeks (FCL or LCL) - Run production-scale batch on real equipment - Compare against historical reference batches - Hold finished product for 30+ day storage stability monitoring - Send finished product samples to key customers for evaluation

Acceptance criteria: - Production-scale parameters match lab batch results - No equipment issues (dispersion, extrusion, application) - Customer feedback positive on finished product - Storage stability acceptable (no settling, no color shift)

Stage 4: First FCL commercial order (Week 7+)

After successful pilot, order a 1 FCL (18–20 t TiO2) commercial volume.

Process: - Place commercial order on new supplier - Receive FCL with full CoA - Use in production parallel with existing supplier (50/50 split typical) - Monitor finished product quality over 1–3 month period - Compare yield, defect rates, customer returns - After successful FCL, transition to 100% new supplier or maintain dual-source

Common pitfalls in qualification:

1. Skipping lab batch: shipping FCL before lab validation often fails — color drift, dispersion issues caught only at production scale 2. Inadequate hold time: 30-day storage stability matters; rushing through and approving immediately misses storage-related issues 3. Comparing CoA only, not application: two TiO2 grades with identical CoA can behave very differently in your specific formulation 4. Single batch validation: validate against 2–3 batches to catch batch-to-batch variation issues 5. Production substitution without lab validation: highest-risk approach; always validate before substituting

Cost of qualification (typical): - Stage 1 sample + CoA review: minimal (sample is free) - Stage 2 lab work: $1000–5000 internal labor + materials - Stage 3 pilot batch: $5000–25000 (TiO2 cost + lab analysis + lost-time on equipment) - Stage 4 first FCL: TiO2 cost + monitoring effort

Total ~$10,000–50,000 for a complete qualification, depending on application complexity. Premium applications (automotive OEM, cosmetic) at the high end.

Payback for cost-down substitution: For a paint plant doing 5000 t/year at 20% TiO2 loading switching from premium-priced TiO2 to SEMITI 996: - TiO2 consumption: 1000 t/year - Cost saving (typical $0.80/kg): $800,000/year - Payback: < 1 month on $50k qualification cost

SEMITI qualification support: - Free samples up to 25 kg - Technical support for lab batch design - On-site visits for premium accounts in Asia - Co-development for complex applications (automotive OEM, premium PVC) - Customer reference program — connect with similar customers who've completed qualification

Application-specific qualification protocols

Different end applications have distinct qualification requirements. Using a generic protocol for a specialized application leads to missed failure modes.

Automotive OEM coatings qualification: Automotive OEM is the most demanding TiO2 qualification because color specification is controlled to ΔE < 0.5 from standard, measured on the full paint system (basecoat + clearcoat) under multiple illuminants (D65, A, F2). Additional OEM-specific tests:

• Bronzing test (ASTM D4086): metallic paint with TiO2 in the basecoat must pass flip-flop color uniformity. TiO2 particle size variation causes bronzing visible at oblique viewing angles.
• Gravelometer chip resistance (SAE J400): not TiO2-specific, but underlies film integrity that depends on TiO2 dispersion quality.
• Ford FLTM BI 160-01 / GM 9984002 weathering: 2000+ hour QUV or Florida exposure with color measurement every 500 hr. Requires chloride rutile with ZrO2 surface treatment.
• Gloss retention at angle: OEM specifies minimum 75% gloss retention at 20° angle after 1000 hr QUV. Sulfate-process TiO2 typically fails this criterion within 600–800 hr.
• Batch-to-batch tolerance documentation: OEM suppliers must demonstrate Cpk ≥ 1.33 on tinting strength and b* over 20+ consecutive production batches. This statistical requirement means qualification is not complete until 20 batches have been delivered and tracked.

Automotive OEM qualification typically takes 6–12 months from sample to approved supplier status. SEMITI 880 (automotive-grade chloride rutile) is specifically engineered for OEM color standards.

Cosmetic / sunscreen qualification: Nano TiO2 for sunscreen requires a different qualification framework from conventional TiO2. The key additional tests versus standard cosmetic ingredients:

• Photocatalytic activity: EFSA methylene blue dye decolorization method (EU requirement for nano UV filters). Target < 5% photocatalytic activity relative to uncoated TiO2 control. SEMITI NANO-30 typically < 2%.
• Primary particle size verification: TEM (transmission electron microscopy) imaging to confirm 15–30 nm primary particle distribution. CoA D50 by laser diffraction measures agglomerates, not primary particles — TEM is the only method that confirms nano classification.
• In vitro SPF: measure Diffey/Robey in vitro SPF at 3 loading levels to build SPF-loading curve for your emulsion system. This predicts in vivo SPF before costly human subject testing.
• 12-week emulsion stability: prepare final formulation, test at 4°C, 25°C, 40°C, and 3 freeze-thaw cycles. TiO2 must not agglomerate or settle beyond redispersible limits.
• Preservative efficacy testing (PET, ISO 11930): nano TiO2 can interfere with some preservative systems. Confirm adequate microbial protection in the final formula.
• Safety assessment: EU Cosmetic Regulation requires a Cosmetic Product Safety Report (CPSR) signed by a qualified safety assessor. SEMITI provides nano TiO2 safety dossier data for inclusion in CPSR.

Pharmaceutical excipient qualification: For TiO2 in tablet film coatings (pharmaceutical grade):

• ICH Q7 GMP audit: the TiO2 supplier must be audited against ICH Q7 (Good Manufacturing Practice for Active Pharmaceutical Ingredients). For excipients, IPEC-PQG GMP guide is the equivalent standard.
• Pharmacopeia compliance: USP <231> or EP 2.4.8 heavy metals test; USP <786> or EP 2.9.31 particle size; USP <735> or EP 2.2.22 XRD for crystal form confirmation.
• Residual solvents: EP 5.4 / ICH Q3C — confirm no Class 1 or Class 2 residual solvents from processing aids.
• Nitrosamine impurity assessment: ICH M7 / ICH S10 — new regulatory requirement (2023–2025) for pharmaceutical excipients. TiO2 manufacturing does not generate nitrosamine precursors, but formal assessment document required.
• Drug master file (DMF): for US FDA submissions, TiO2 used in drug products should have a Type IV DMF filed by the supplier. SEMITI NANO-30 DMF available for pharma-grade cosmetic sunscreen applications; contact us for pharmaceutical grade DMF arrangements.