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HJ 694-2014 (HJ694-2014)

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BASIC DATA
Standard ID HJ 694-2014 (HJ694-2014)
Description (Translated English) Water Quality - Determination of Mercury, Arsenic, Selenium, Bismuth and Antimony - Atomic Fluorescence Spectrometry
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z16
Word Count Estimation 16,125
Date of Issue 2014/3/13
Date of Implementation 2014/7/1
Quoted Standard GB/T 21191; HJ/T 91; HJ/T 164; HJ 493; HJ 494
Drafting Organization Nanjing Environmental Monitoring Center Station
Administrative Organization Department of Environmental Protection
Regulation (derived from) Ministry of Environmental Protection Notice No. 17 of 2014
Issuing agency(ies) Ministry of Environmental Protection
Summary This Standard specifies the Determination of mercury, arsenic, selenium and antimony secret atomic fluorescence spectrometry. This Standard applies to surface water, groundwater measurement, sewage and industrial waste mercury, arsenic, selenium, antimony


HJ 694-2014: PDF in English
HJ 694-2014
HJ
NATIONAL ENVIRONMENTAL PROTECTION STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
Water Quality - Determination of Mercury, Arsenic,
Selenium, Bismuth and Antimony –
Atomic Fluorescence Spectrometry
ISSUED ON: MARCH 13, 2014
IMPLEMENTED ON: JULY 01, 2014
Issued by: Ministry of Environmental Protection
Table of Contents
Announcement ... 3 
Foreword ... 4 
1 Application scope ... 5 
2 Normative references ... 5 
3 Terms and definitions ... 6 
4 Principle of the method ... 6 
5 Interference and elimination ... 6 
6 Reagents and materials ... 7 
7 Instruments and equipment ... 11 
8 Samples ... 11 
9 Analysis steps ... 12 
10 Result calculation and representation ... 15 
11 Precision and accuracy ... 15 
12 Quality assurance and quality control ... 17 
13 Waste disposal ... 18 
14 Notes ... 18 
Annex A ... 19 
Announcement
2014 No. 17
Ministry of Environmental Protection of the People's Republic of China
To implement the “Environmental Protection Law of the People's Republic of China”,
protect the environment, protect human health, and regulate environmental
monitoring, two standards, including “Water Quality - Determination of Mercury,
Arsenic, Selenium, Bismuth and Antimony - Atomic Fluorescence Spectrometry”, are
approved as national environmental protection standards, and are published.
The standard names and numbers are as follows:
1. “Water Quality - Determination of Mercury, Arsenic, Selenium, Bismuth and
Antimony - Atomic Fluorescence Spectrometry” (HJ 694-2014);
2. “Soil - Determination of organic carbon - Combustion oxidation nondispersive
infrared absorption method” (HJ 695-2014).
Above standards are implemented since July 1, 2014, and are published by China
Environmental Press. The standard content can be inquired at the website of the
Ministry of Environmental Protection (bz.mep.gov.cn).
Notice is hereby given.
Ministry of Environmental Protection
March 13, 2014
Foreword
To implement the “Environmental Protection Law of the People's Republic of China”
and "Water Pollution Prevention Law of the People's Republic of China”, protect the
environment, protect human health, and regulate the monitoring methods of mercury,
arsenic, selenium, antimony, and bismuth in water, this Standard is formulated.
This Standard specifies the atomic fluorescence spectrometry for determination of
mercury, arsenic, selenium, bismuth, and antimony in water.
This Standard is released for the first time.
Annex A of this Standard is informative.
This Standard was formulated by the Department of Science, Technology and
Standards of Ministry of Environment Protection.
Main drafting organization of this Standard: Nanjing Environmental Monitoring Center.
Verification organizations of this Standard: Jiangsu Environment Monitoring Center,
Jiangsu Physical and Chemical Testing Center, Wuxi Environmental Monitoring
Center Station, Changzhou Environmental Monitoring Center, Zhenjiang
Environmental Monitoring Center Station, and Taizhou Environmental Monitoring
Center.
This Standard was approved by the Ministry of Environmental Protection on March 13,
2014.
This Standard shall be implemented from July 1, 2014.
This Standard shall be interpreted by the Ministry of Environmental Protection.
Water Quality - Determination of Mercury, Arsenic,
Selenium, Bismuth and Antimony –
Atomic Fluorescence Spectrometry
Warning: nitric acid, hydrochloric acid, and perchloric acid have a strong
corrosivity and a strong oxidability, so it shall wear protective equipment when
operating, so as to avoid contact with skin and clothing. The pretreatment
process of all samples shall be carried out in a fume hood.
1 Application scope
This Standard specifies the atomic fluorescence spectrometry for the determination of
mercury, arsenic, selenium, bismuth, and antimony in water.
This Standard applies to the determination of soluble [Translator: dissolved-state] and
total quantity of mercury, arsenic, selenium, bismuth, and antimony in surface water,
groundwater, sewage, and industrial waste water.
According to the method of this Standard, the detection limit of mercury is 0.04μg/L,
the determination lower limit of mercury is 0.16μg/L; the detection limit of arsenic is
0.3μg/L, the determination lower limit of arsenic is 1.2μg/L; the detection limit of
selenium is 0.4μg/L, the determination lower limit of selenium is 1.6μg/L; the detection
limit of bismuth and antimony is 0.2μg/L, the determination lower limit of bismuth is
0.8μg/L.
2 Normative references
This Standard references the following documents or its terms. For undated
references, the latest version applies to this Standard.
GB/T 21191 Atomic fluorescence spectrometer
HJ/T 91 Technical specifications requirements for monitoring of surface water
and waste water
HJ/T 164 Technical specifications for environmental monitoring of groundwater
HJ 493 Water quality - Technical regulation of the preservation and handling of
samples
HJ 494 Water quality - Guidance on sampling techniques
3 Terms and definitions
The following terms and definitions apply to this Standard.
3.1
Soluble mercury, arsenic, selenium, bismuth and antimony
It refers to the content of mercury, arsenic, selenium, bismuth, and antimony
determined in the filtrate of the not-acidified sample, after being filtered through the
filter membrane with a pore size of 0.45μg.
3.2
Total quantity of mercury, arsenic, selenium, bismuth and antimony
It refers to the content of mercury, arsenic, selenium, bismuth, and antimony
determined in the unfiltered sample, after being dissolved.
3.3
Determined elements
It refers to mercury, arsenic, selenium, bismuth, and antimony elements.
4 Principle of the method
The test solution after pretreatment is put into the atomic fluorescence spectrometer;
under potassium borohydride (or sodium borohydride)’s reducing effects at acidic
conditions, it generates arsine, bismuthine, antimony hydrogen, hydrogen selenide,
and mercury atoms; the hydride forms ground-state atoms in argon and hydrogen
flames; its ground-state atoms and mercury atoms generate atomic fluorescence by
the excitation of the light emitted by element (mercury, arsenic, selenium, bismuth,
and antimony) lights; the atomic fluorescence intensity is in direct proportion to the
content of determined elements in the sample solution within a certain range.
5 Interference and elimination
5.1 The elements in acidic medium, that can react with potassium borohydride and
generate hydride, would affect each other and produce interference; adding thiourea
+ ascorbic acid solution (6.20) can substantially eliminate the interference.
5.2 Copper and other transition metals that are above a certain concentration may
interfere to the determination; adding thiourea + ascorbic acid solution (6.20) can
eliminate most of the interference. Under the experimental conditions of this Standard,
samples containing less than 100mg/L of Cu2+, less than 50mg/L of Fe2+, less than
1mg/L of Co2+, less than 10mg/L of Pb2+ (5mg/L for selenium), and less than 150mg/L
of Mn2+ (2mg/L for selenium) do not affect the determination.
5.3 Common anions do not interfere to the determination.
5.4 Physical interference elimination. Select two-layer-structure quartz tube atomizer;
with the outer and inner layers filled with argon gas, form a protective outer layer to
isolate air, so that the ground-state atom of determined elements do not collide with
oxygen and nitrogen in the air, so as to reduce the fluorescence quenching effect on
the determination.
6 Reagents and materials
Unless otherwise indicated, use analytically chemical reagents that comply with
national standards when analyzing, water for test is freshly prepared deionized or
distilled water.
6.1 Hydrochloric acid: ρ(HCl) = 1.19g/ml, guarantee reagent.
6.2 Nitric acid: ρ(HNO3) = 1.42g/ml, guarantee reagent.
6.3 Perchloric acid: ρ(HClO4) = 1.68g/ml, guarantee reagent.
6.4 Hydrogen sodium hydride (NaOH).
6.5 Potassium borohydride (KBH4).
6.6 Thiourea (CH4N2S).
6.7 Ascorbic acid (C6H8O6).
6.8 Potassium dichromate (K2Cr2O7): guarantee reagent.
6.9 Mercuric chloride (HgCl2): guarantee reagent.
6.10 Arsenic trioxide (As2O3): guarantee reagent.
6.11 Selenium powder: high-purity (the mass fraction is more than 99.99%).
6.12 Bismuth: high-purity (the mass fraction is more than 99.99%).
6.13 Antimony trioxide (Sb2O3), guarantee reagent.
6.14 Hydrochloric acid solution: 1 + 1.
6.15 Hydrochloric acid solution: 5 + 95.
6.16 Nitric acid solution: 1 + 1.
6.17 Hydrochloric acid - nitric acid solution
Weigh 300ml of hydrochloric acid (6.1) and 100ml of nitrate (6.2) respectively; add to
400ml of water; mix well.
6.18 Mixture acid of nitric acid - perchloric acid
Prepare by mixing an equal volumes of nitric acid (6.2) and perchloric acid (6.3).
Prepare it when it is to be used.
6.19 Reducing agents
6.19.1 Potassium borohydride Solut......