1.Verification Overview
Objective of validation
To verify the lab applicability of ICP-OES for metal elements in ambient air & exhaust particulates. Instrument conditions, calibration curve, MDL, LOQ, precision, accuracy and real-sample test were systematically validated to meet HJ 777-2015 requirements.
2.Validation Basis
HJ 777-2015, Determination of Metals in Ambient Air and Exhaust Gas Particulates by Inductively Coupled Plasma-Optical Emission Spectrometry
JJG 768, Verification Regulation for Emission Spectrometers
GB/T 27404, General Rules for Chemical-analytical Method Validation
3. Main Instruments
1.ICP-OES,Model ICP-6810-A2,Shanghai Macylab Instrument Inc.
2.Microwave digester
3.Electronic balance
4.Air particulate sampler
Instrument key parameters：
Source: Solid-state RF generator, 27.12 MHz
Torch: Vertical torch, cold-cone tail-flame removal
Detector: High-speed array CCD, full-spectrum direct readout with single exposure
Nebulizer system: MFC for carrier, auxiliary & coolant gas
Linear range: Wide dynamic range, trace-to-major analysis
4.Validation Items & Results
4.1 Optimization of Instrument Conditions
RF Power: 1300 W, optimized per sample matrix Nebulizer gas flow: 0.65 L/min, controlled by MFC Auxiliary gas flow: 1.20 L/min, stabilize plasma Coolant gas flow: 15.00 L/min, protect torch Observation height: 15 mm, optimized for vertical torch
Integration time: 3s, ensure SNR
Replicate measurements: 3 replicates, average taken
4.2 Calibration Curve Validation
Standard solution preparation: Certified reference materials used for multi-element mixed standards. Gradient: 0、0.5、1.0、2.0、5.0、10.0 μg/L。
容不要变动
| Elem | Wave.(nm) | Linear(μg/L) | r(r) | Intercept |
|---|---|---|---|---|
| Al | 396.152 | 0.5~10.0 | 0.9998 | 0.0012 |
| As | 193.696 | 0.5~10.0 | 0.9996 | 0.0008 |
| Cd | 228.802 | 0.5~10.0 | 0.9997 | 0.0010 |
| Cr | 267.716 | 0.5~10.0 | 0.9995 | 0.0015 |
| Cu | 324.754 | 0.5~10.0 | 0.9998 | 0.0009 |
| Fe | 238.204 | 0.5~10.0 | 0.9997 | 0.0011 |
| Mn | 257.610 | 0.5~10.0 | 0.9996 | 0.0013 |
| Pb | 220.353 | 0.5~10.0 | 0.9995 | 0.0014 |
| Zn | 213.856 | 0.5~10.0 | 0.9998 | 0.0007 |
Conclusion: r≥0.9995 for all elements, meets HJ 777-2015
4.3 MDL & LOQ
Calculated per HJ 777-2015 Appendix A, sampling volume 150 m³, final volume 50 mL. MDL = 3×blank SD；LOQ = 10×blank SD
| Elem | MDL(μg/L) | LOQ(μg/L) | MDL(mg/kg) | LOQ(mg/kg) |
|---|---|---|---|---|
| Al | 0.05 | 0.17 | 0.003 | 0.010 |
| As | 0.02 | 0.07 | 0.001 | 0.004 |
| Cd | 0.01 | 0.03 | 0.001 | 0.002 |
| Cr | 0.02 | 0.07 | 0.001 | 0.004 |
| Cu | 0.02 | 0.07 | 0.001 | 0.004 |
| Fe | 0.10 | 0.33 | 0.006 | 0.020 |
| Mn | 0.02 | 0.07 | 0.001 | 0.004 |
| Pb | 0.02 | 0.07 | 0.001 | 0.004 |
| Zn | 0.03 | 0.10 | 0.002 | 0.006 |
Conclusion: MDL & LOQ meet HJ 777 2015 requirements
4.4 Precision (Low Med High levels)
Certified filter-membrane reference materials, 6 replicates per level
| Level | Elem. | Spiked(μg/L) | result(μg/L) | Mean(μg/L) | standard(SD) | RSD(%) |
|---|---|---|---|---|---|---|
| Low | As | 0.5 | 0.48, 0.51, 0.49, 0.50, 0.52, 0.49 | 0.50 | 0.015 | 3.0 |
| Cd | 0.5 | 0.49, 0.50, 0.51, 0.48, 0.50, 0.49 | 0.495 | 0.011 | 2.2 | |
| Pb | 0.5 | 0.51, 0.49, 0.50, 0.52, 0.48, 0.50 | 0.50 | 0.014 | 2.8 | |
| Mid | As | 2.0 | 1.98, 2.02, 2.01, 1.99, 2.00, 2.01 | 2.00 | 0.014 | 0.7 |
| Cd | 2.0 | 1.99, 2.01, 2.00, 2.02, 1.98, 2.00 | 2.00 | 0.014 | 0.7 | |
| Pb | 2.0 | 2.01, 1.99, 2.00, 2.02, 1.98, 2.00 | 2.00 | 0.014 | 0.7 | |
| High | As | 5.0 | 4.98, 5.02, 5.01, 4.99, 5.00, 5.01 | 5.00 | 0.014 | 0.3 |
| Cd | 5.0 | 4.99, 5.01, 5.00, 5.02, 4.98, 5.00 | 5.00 | 0.014 | 0.3 | |
| Pb | 5.0 | 5.01, 4.99, 5.00, 5.02, 4.98, 5.00 | 5.00 | 0.014 | 0.3 |
Precision Criteria： RSD ≤ 10%（low level），RSD ≤ 5%（Medium/High level）
Conclusion: All-level RSD complies with requirements; good precision achieved.
4.5 Trueness (Spike Recovery)
Certified filter-membrane metal reference materials, spike-recovery method applied.
| Level | Elem. | Background(μg/L) | Spiked(μg/L) | Measured(μg/L) | Rec.(%) | Avg Rec.(%) |
|---|---|---|---|---|---|---|
| Low | As | 0.10 | 0.50 | 0.59 | 98.0 | 97.5 |
| Cd | 0.05 | 0.50 | 0.54 | 98.0 | 97.8 | |
| Pb | 0.08 | 0.50 | 0.57 | 98.0 | 97.6 | |
| Mid | As | 0.50 | 2.00 | 2.48 | 99.0 | 98.8 |
| Cd | 0.10 | 2.00 | 2.09 | 99.5 | 99.2 | |
| Pb | 0.15 | 2.00 | 2.14 | 99.5 | 99.3 | |
| High | As | 1.00 | 5.00 | 5.98 | 99.6 | 99.4 |
| Cd | 0.20 | 5.00 | 5.19 | 99.8 | 99.6 | |
| Pb | 0.30 | 5.00 | 5.28 | 99.6 | 99.5 |
Criterion: Recovery 90%-110%
Conclusion: All recoveries 97.5%-99.8%, good trueness
4.6 Real Sample Test
Samples: Ambient air PM10 filter membranes
| SampleID | Elem. | Meas.(μg/L) | Converted(mg/kg) | Remarks |
|---|---|---|---|---|
| 001 | Al | 12.5 | 0.83 | 50ml final volume |
| Fe | 45.2 | 3.01 | ||
| Mn | 2.1 | 0.14 | ||
| Pb | 0.8 | 0.05 | ||
| 002 | Al | 15.8 | 1.05 | 50ml final volume |
| Fe | 52.3 | 3.49 | ||
| Mn | 2.5 | 0.17 | ||
| Pb | 1.2 | 0.08 |
Conclusion: Real-sample results are reasonable. The method is suitable for metal analysis of ambient air particulate matter.
5.Interferences and Elimination
According to HJ 777-2015, main interferences for ICP-OES are listed below:
| Type | Source | Elimination |
|---|---|---|
| Spectral | Background, line overlap | Background correction, interference coefficient, matrix matching |
| Non-spectral | Chemical / ionization / physical | Dilution, releasing agent, internal standard |
Lab measures：
Matrix-matched standards
Dilute high-salt samples
Select low-interference wavelengths
Cold-cone tail-flame removal for self-absorption reduction
6.QA/QC
| Item | Requirement | Implementation |
|---|---|---|
| Blank test | Blank < MDL | Done, compliant |
| Duplicate test | Rel. dev. ≤10% | Done, compliant |
| CRM check | Within certified range | Done, compliant |
| Spike recovery | 90%~110% | Done, compliant |
| Calibration curve | r≥0.999 | Done，r≥0.9995 |
7.Verification Conclusion
Systematic verification of ICP-6810-A2 for metals in ambient & waste-gas particulates:
| Item | Result | Compliance |
|---|---|---|
| Instrument | Reasonable settings, stable | ✓ Yes |
| Calibration curve | r≥0.9995 | ✓ Yes |
| MDL | HJ 777-2015 Appendix A | ✓ Yes |
| LOQ | HJ 777-2015 Appendix A | ✓ Yes |
| Precision | RSD ≤3.0%(low), ≤0.7%(med-high) | ✓ Yes |
| Trueness | Recovery 97.5%~99.8% | ✓ Yes |
| Real sample | Valid for routine use | ✓ Yes |
Overall: Stable laboratory performance, meets HJ 777-2015. Verification passed, suitable for metal analysis of ambient-air and waste-gas particulates.
8. Document Information
Validation Organization: Shanghai Macylab Instrument Inc.
Report No.: MACY-2026-0727
Document Code: 20260726-ICP6810CN
Validation Date: July 26, 2026
This application validation report is applicable to the samples and test conditions described in this document. Reproduction or distribution of this report, in whole or in part, requires prior written authorization from Shanghai Macylab Instrument Inc.
The information provided in this document is for reference purposes. Specifications and technical information are subject to change without prior notice.
2026 Shanghai Macylab Instrument Inc. All rights reserved.
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