1.Verification Overview
1.1 Purpose
Method verification for MACY ICP-6810-A2 ICP-OES per HJ 776-2015, to verify instrument performance, applicability and detection capacity.
1.2 Reference
HJ 776-2015《Water quality-Determination of 32 elements-ICP-OES》
1.3 Analytes
32 elements: Ag、Al、As、B、Ba、Be、Ca、Cd、Co、Cr、Cu、Fe、K、Mg、Mn、Mo、Na、Ni、P、Pb、S、Sb、Se、Si、Sn、Sr、Ti、Tl、V、Zn、Li、W
1.4 Content
Instrument parameters, calibration curve, MDL, LOQ, precision, trueness, real-sample spike-recovery test
2.Instruments and Reagents
2.1 Main Instruments
Inductively Coupled Plasma Optical Emission Spectrometer：Macy ICP-6810-A2
Electronic balance: precision 0.1 mg
Ultrapure water machine：resistivity≥18.2 MΩ·cm
pH meter: precision 0.01 pH
Microwave digester: used as supporting equipment
Glassware such as volumetric flasks and pipettes: Class A
2.2 Main Reagents & Reference Materials
Nitric acid(GR), Hydrochloric acid(GR), Hydrofluoric acid(GR)
32-element mixed standard solution (1000 mg/L)
National water CRM GBW(E)080546 (surface water)
National water CRM GBW(E)080547 (groundwater）
National water CRM GBW(E)080548 (domestic sewage)
Internal standard solution（Sc、Y、In、Re）
3.Instrument Conditions
3.1 ICP-OES Parameters
RF Power: 1400 W
Plasma gas: 15.0 L/min
Auxiliary gas: 0.2 L/min
Nebulizer gas: 0.65 L/min
Nebulizer: concentric
Spray chamber: dual-channel cyclonic
Observation height: 15 mm
Integration time: 3 s/point
Wavelength: 190-800 nm
Lamp current: 12 mA
Negative HV: 800 V
Sampling depth: 6 mm
Cooling-water: 12 L/min
Ignition: gas on first, then ignite
4.Calibration Curve
4.1 Standard Series Preparation
Single-point or multi-point calibration for 32-element mixed standard solutions：
Low-concentration series：0.005、0.010、0.020、0.050、0.100 mg/L
High-concentration series：0.200、0.500、1.000、2.000、4.000 mg/L
Internal standard solution：Sc 10 mg/L、Y 10 mg/L、In 10 mg/L、Re 10 mg/L
4.2 Calibration Curve Results
Good linearity for all 32 elements, r ≥ 0.999, complying with HJ 776-2015
Examples：
Al: y=1234.5x+0.023, r=0.9998, linear range 0.01-4.00 mg/L
Fe: y=5678.9x+0.045, r=0.9999, linear range 0.01-4.00 mg/L
Cu: y=2345.6x+0.012, r=0.9997, linear range 0.005-2.00 mg/L
Zn: y=3456.7x+0.034, r=0.9998, linear range 0.005-2.00 mg/L
Pb: y=1567.8x+0.021, r=0.9996, linear range 0.005-1.00 mg/L
5.Limit of Detection & Limit of Quantitation
5.1 Test Method
Per HJ 776-2015: LOD = 3×blank standard deviation; LOQ = 10×blank standard deviation.Measure 7 blank replicates for 32 elements, calculate standard deviation to obtain LOD and LOQ.5.2 LOD & LOQ Results (Partial Elements)
| Element | LOD(mg/L) | LOQ(mg/L) |
|---|---|---|
| Ag | 0.002 | 0.007 |
| Al | 0.005 | 0.017 |
| As | 0.001 | 0.003 |
| B | 0.01 | 0.033 |
| Ba | 0.003 | 0.01 |
| Be | 0.0005 | 0.002 |
| Ca | 0.05 | 0.167 |
| Cd | 0.0003 | 0.001 |
| Co | 0.0005 | 0.002 |
| Cr | 0.001 | 0.003 |
| Cu | 0.001 | 0.003 |
| Fe | 0.01 | 0.033 |
| K | 0.02 | 0.067 |
| Mg | 0.02 | 0.067 |
| Mn | 0.0005 | 0.002 |
| Mo | 0.0005 | 0.002 |
| Na | 0.03 | 0.1 |
| Ni | 0.001 | 0.003 |
| P | 0.005 | 0.017 |
| Pb | 0.001 | 0.003 |
| S | 0.1 | 0.333 |
| Sb | 0.0005 | 0.002 |
| Se | 0.0005 | 0.002 |
| Si | 0.05 | 0.167 |
| Sn | 0.001 | 0.003 |
| Sr | 0.002 | 0.007 |
| Ti | 0.001 | 0.003 |
| Tl | 0.0002 | 0.001 |
| V | 0.001 | 0.003 |
| Zn | 0.001 | 0.003 |
| Li | 0.0005 | 0.002 |
| W | 0.0005 | 0.002 |
All method detection limits (MDLs) and limits of quantification (LOQs) for all elements meet the requirements of HJ 776-2015, demonstrating that the method sensitivity meets the specified requirements.
6.Precision Verification
6.1 Test Scheme
Per HJ 776-2015, precision test at low, medium and high concentration levels:
Low: approx. 3 × LOD
Medium: 0.500 mg/L
High: 4.000 mg/L
Each concentration level was prepared into 7 parallel samples for full-procedure measurement, and relative standard deviation (RSD) was calculated.
6.2 Precision Verification Results (Partial Elements)
| Level | Al | Fe | Cu | Zn | Pb |
| Low Conc. | 2.30% | 3.10% | 2.80% | 2.50% | 3.40% |
| Mid Conc. | 1.20% | 1.50% | 1.30% | 1.40% | 1.60% |
| High Conc. | 0.80% | 0.90% | 0.70% | 0.80% | 1.00% |
RSD of all 32 elements at three conc. levels ≤5% (≤10% for low conc.), satisfying the precision requirement of HJ 776-2015 (RSD ≤5%).
7.Accuracy Verification
7.1 Test Scheme
National water-quality certified reference materials (CRMs) were used for accuracy verification：
GBW(E)080546 Surface-water CRM
GBW(E)080547 Groundwater CRM
GBW(E)080548 Domestic-sewage CRM
Each CRM was independently prepared at three conc. levels (low, medium, high). Each level was measured 7 times to calculate relative error (RE).
7.2 Accuracy Test Results of CRMs (Partial Elements)
| CRM | Elem | Cert.(mg/L) | Meas.(mg/L) | RE |
| GBW(E)080546 | Al | 12.5 | 12.3 | -1.60% |
| GBW(E)080546 | Fe | 45.2 | 44.8 | -0.90% |
| GBW(E)080546 | Cu | 2.35 | 2.38 | 1.30% |
| GBW(E)080546 | Zn | 8.45 | 8.52 | 0.80% |
| GBW(E)080547 | Al | 8.2 | 8.1 | -1.20% |
| GBW(E)080547 | Fe | 12.5 | 12.3 | -1.60% |
| GBW(E)080547 | Cu | 1.15 | 1.18 | 2.60% |
| GBW(E)080547 | Zn | 3.25 | 3.28 | 0.90% |
| GBW(E)080548 | Al | 25.8 | 25.5 | -1.20% |
| GBW(E)080548 | Fe | 78.5 | 77.8 | -0.90% |
| GBW(E)080548 | Cu | 4.25 | 4.32 | 1.60% |
| GBW(E)080548 | Zn | 15.6 | 15.8 | 1.30% |
All RE values of CRMs are within ±10%, meeting HJ 776-2015 requirement (RE ≤ ±15%).
8. Spiked-Recovery Verification
8.1 Test Scheme
Four real-world water samples：
surface water(river)
roundwater(well)
domestic sewage(WWTP)
industrial wastewater(electroplating plant)
Blank, original and spiked tests (spike:1-2×orig. conc.), 3 replicates per sample.
8.2 Spiked-Recovery Results (Partial Elem.)
| Sample | Elem | Orig(mg/L) | Spiked(mg/L) | Rec |
| Surface Water | Al | 0.12 | 0.52 | 88.50% |
| Surface Water | Fe | 0.45 | 1.25 | 92.30% |
| Surface Water | Cu | 0.08 | 0.25 | 95.20% |
| Groundwater | Al | 0.05 | 0.28 | 91.80% |
| Groundwater | Fe | 0.15 | 0.52 | 89.50% |
| Groundwater | Zn | 0.03 | 0.15 | 93.20% |
| Domestic sewage | Al | 2.35 | 6.85 | 90.80% |
| Domestic sewage | Fe | 8.52 | 18.25 | 88.90% |
| Domestic sewage | Cu | 0.45 | 1.28 | 92.50% |
| Industrial wastewater | Al | 12.5 | 35.8 | 91.20% |
| Industrial wastewater | Fe | 45.2 | 125.5 | 89.80% |
| Industrial wastewater | Cu | 8.25 | 22.5 | 93.50% |
| Industrial wastewater | Zn | 15.6 | 42.8 | 90.50% |
All recoveries 80%-120%, complying with HJ 776-2015, reliable method accuracy.
9. Sample Preparation Procedure
9.1 Sample Collection & Preservation
Collect water samples with clean PE bottles, rinse 3 times before sampling.
Acidify with HNO₃ to pH＜2 immediately after sampling.
Store at 4 ℃, finish test within 24 h. Avoid direct sunlight & sharp temperature change during transport.
9.2 Sample Pretreatment
Clear samples: use supernatant directlyTurbid samples: filter with 0.45 μm membrane
Suspended-matter samples: microwave digestion Transfer 10.00 mL sample into digestion tank, add 5 mL HNO-, 1 mL HF.
Microwave program: 120 ℃/10 min →160 ℃/15 min →180 ℃/20 min.
Cool, transfer and dilute to 50 mL. Run blank test simultaneously.
9.3 Instrument Measurement
Warm-up for 30 min, ignite plasma and stabilize 15 min.
Calibrate instrument with standard curve solutions.
Test blank, standard series and sample solutions sequentially.
Insert QC sample per 10 samples; correct drift regularly with internal-standard solution
10.Validation Conclusion
10.1 Instrument Condition Validation
MACYLAB ICP-6810-A2 ICP-OES operates with reasonable parameters and stable performance, complying with HJ 776-2015.
10.2 Calibration Curve Validation
Good linearity for 32 elements, correlation coefficient r ≥0.999. Linear range covers real-sample concentrations, meeting standard requirements.
10.3 LOD & LOQ Validation
LOD and LOQ of 32 elements meet or exceed HJ 776-2015, sufficient sensitivity for water quality analysis.
10.4 Precision Validation
RSD ≤5% for low-/mid-/high-level concentrations (≤10% for low concentration), satisfying HJ 776-2015 precision criteria.
10.5 Trueness Validation
3 national water-quality CRMs tested; all RE within ±10%, complying with HJ 776-2015 (RE ≤ ±15%).
10.6 Real-Sample Spiked Recovery Validation
Recoveries of four sample types range 80%-120%, proving reliable method trueness.
10.7 Whole-Process Sample Preparation Validation
Standardized workflow from sampling, preservation, pretreatment to instrumental measurement with reliable results.
Overall Conclusion: When determining 32 elements in water per HJ 776-2015, MACYLAB ICP-6810-A2 ICP-OES passes all validation indexes. The method is qualified and applicable for real-sample testing.
11.Document Information
Validation Organization: Shanghai Macylab Instrument Inc.
Report No.: MACY-2026-0828
Document Code: 20260831-ICP6810CN
Validation Date: August 28, 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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