HJ 1268-2022 in English

VALID

Water quality-Determination of methyl mercury and ethyl mercury-Liquid chromatography - atomic fluorescence spectrometry

Issued on:2022-12-12
Implemented on:2023-06-15
File Format:PDF
Delivery:Via email within 1~3 business days

Price(USD)： $180.00
$175.00

Standard No:	HJ 1268-2022
Document status:	VALID
Title in English:	Water quality-Determination of methyl mercury and ethyl mercury-Liquid chromatography - atomic fluorescence spectrometry
Title in Chinese:	水质甲基汞和乙基汞的测定液相色谱-原子荧光法
Language:	English
File Format:	Electronic (PDF)
Delivery:	Via email within 1~3 business days
Issued on:	2022-12-12
Implemented on:	2023-06-15
Professional Classification:	HJ-Environment
Related Keywords:	water quality-determination water sample→40ml dichloromethane extraction atomic fluorescence spectrometry introduction analysis surface water environmental quality standards liquid chromatography-atomic fluorescence spectrometry
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本标准规定了测定水中甲基汞和乙基汞的液相色谱-原子荧光法。
本标准适用于地表水、地下水、生活污水、工业废水和海水中甲基汞和乙基汞的测定。
取样体积为 1 L，反萃取液体积为 3.0 ml，进样体积为 100 μl 时，方法检出限为 0.08 ng/L～0.1 ng/L，测定下限为 0.32 ng/L～0.4 ng/L。详见附录 A。

Introduction

Analysis of standard technology

This standard establishes for the first time a standardized method for the determination of methylmercury and ethylmercury in water by liquid chromatography-atomic fluorescence spectrometry (LC-AFS), and innovatively adopts an L-cysteine complex extraction system to achieve efficient separation and ultra-trace detection of organic mercury forms.

In-depth analysis of the principle of the method

The technical route includes three key steps: dichloromethane extraction → L-cysteine back extraction → online ultraviolet digestion-atomic fluorescence detection. The chromatographic separation uses a C18 reverse phase column, and the mobile phase contains a methanol-water system (80:20, v/v) containing 1.2g/L L-cysteine and 0.62g/L ammonium acetate.

Comparison of key parameters

Analyte	Detection limit (ng/L)	Lower limit of determination (ng/L)	Retention time (min)	Recovery range
Methylmercury	0.08	0.32	3.2-3.8	68.7-109%
Ethylmercury	0.10	0.40	4.5-5.2	66.8-109%

Instrument configuration requirements

Core equipment needs to be equipped with: Liquid chromatography system (C18 chromatographic column, 5μm×150mm×4.6mm), Online ultraviolet digestion device (254nm ultraviolet lamp), Atomic fluorescence spectrometer (mercury hollow cathode lamp). The purity of argon gas must be ≥99.999%.

Key points of sample pretreatment

Storage conditions: pH1-2 environment, 4℃ protected from light, add 2ml saturated copper sulfate solution
Extraction process: 1L water sample→40ml dichloromethane extraction (repeat 3 times)→anhydrous sodium sulfate dehydration→3ml back extraction solution (containing 1% L-cysteine)
Demulsification method: Centrifugation, freezing or glass wool filtration can be used for emulsification

Quality assurance system

Standards establish strict quality control requirements:

Blank test is required for each batch of samples (＜MDL)
Correlation coefficient of standard curve ≥0.995
Relative deviation of parallel samples ≤30%
Matrix spike recovery rate 65-120%

Recommendations for the implementation of the standard

Key points for application in different water types:

Water type	Special treatment	Shelf life
Seawater	No need to add sodium chloride	3 days
Industrial wastewater	Pay attention to matrix interference	3 days
Only measure methylmercury	Can be extended to 8 days	8 days

Technology evolution analysis

Compared with the traditional GC-ECD method, the LC-AFS technology of this standard has the following advantages: no derivatization required, avoiding mercury loss, good morphological specificity, etc. The detection limit of the method is one order of magnitude lower than that of EPA 1630, meeting the mercury limit requirement (≤50ng/L) in my country's "Surface Water Environmental Quality Standards".

More samples: JJG 21-2008 DL/T 5154-2012 QC/T 942-2021

Sample only — not a preview of HJ 1268-2022