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HJ 694-2014: Water Quality - Determination of Mercury, Arsenic, Selenium, Bismuth and Antimony - Atomic Fluorescence Spectrometry
HJ 694-2014
Water Quality - Determination of Mercury, Arsenic, Selenium, Bismuth and Antimony - Atomic Fluorescence Spectrometry
People's Republic of China National Environmental Protection Standards
Water quality - Determination of mercury, arsenic, selenium, bismuth and antimony
Atomic Fluorescence Spectrometry
Water Quality-Determination of Mercury, Arsenic, Selenium, Bismuth
and Antimony -Atomic Fluorescence Spectrometry
(Release)
Issued on.2014-03-13
2014-07-01 implementation
Issued by the Ministry of Environmental Protection
Table of Contents
Preface .II
1. Scope ..1
2 Normative references .1
3 Terms and Definitions .1
4 principle of the method ..1
5 eliminate interference and 2
6 Reagents and materials .2
7 .4 instruments and equipment
8 samples .5
Analysis Step 9 ..5
10 Results Calculation and representation .7
11 precision and accuracy .7
12 Quality assurance and quality control ..9
13 waste disposal ..9
14 Note ..9
Appendix A 10
Foreword
To implement the "People's Republic of China Environmental Protection Law" and "People's Republic of China Water Pollution Prevention Law" to protect the environment,
Protection of human health, regulate water mercury, arsenic, selenium, antimony and bismuth monitoring methods, the development of this standard.
This standard specifies the Determination of mercury, arsenic, selenium, bismuth and antimony atomic fluorescence spectrometry.
This standard is the first release.
Appendix A of this standard is an informative annex.
This standard is developed by the Ministry of Environmental Protection Science, Technology organization.
This standard is mainly drafted by. Nanjing Environmental Monitoring Center.
The standard verification. Jiangsu Provincial Environmental Monitoring Center, physical and chemical testing center in Jiangsu Province, Wuxi City Environmental Monitoring Center,
Changzhou Municipal Environmental Monitoring Center, Zhenjiang Municipal Environmental Monitoring Center Station and Taizhou Municipal Environmental Monitoring Center.
This standard MEP March 13, 2014 for approval.
This standard from July 1, 2014 implementation.
The standard explanation by the Ministry of Environmental Protection.
Water mercury, arsenic, selenium, bismuth and antimony Atomic Fluorescence Spectrometry
Warning. nitric acid, hydrochloric acid and perchloric acid is highly corrosive and strong oxidizing, the operation should wear protective equipment to avoid contact
Touch skin and clothing. Pretreatment All samples should be carried out in a fume hood.
1 Scope
This standard specifies the Determination of mercury, arsenic, selenium, bismuth and antimony atomic fluorescence spectrometry.
This standard applies to surface water, groundwater and dissolved, domestic sewage and industrial wastewater mercury, arsenic, selenium, bismuth and antimony
Determination of the total.
The standard method of mercury detection limit was 0.04μg/L, detection limit is 0.16μg/L; arsenic detection limit of 0.3μg/L, measured
The lower limit was 1.2μg/L; selenium detection limit of 0.4μg/L, detection limit 1.6μg/L; bismuth and antimony detection limit was 0.2μg/L, measured
The lower limit of 0.8μg/L.
2 Normative references
This standard refers to the contents of the following documents or the terms. For undated references, the effective version suitable
For this standard.
GB/T 21191 atomic fluorescence spectrometer
HJ/T 91 surface water and wastewater monitoring technical specifications
HJ/T 164 groundwater environmental monitoring technical specifications
Conservation and management of technical regulations HJ 493 water quality samples
HJ 494 Water Sampling technical guidance
3 Terms and Definitions
The following terms and definitions apply to this standard.
3.1 dissolved mercury, arsenic, selenium, bismuth and antimony
soluble mercury, arsenic, selenium, bismuth and antimony
Means without mercury, arsenic, selenium, bismuth and antimony content of the samples after acidification of 0.45μm pore size membrane filter was measured.
3.2 mercury, arsenic, selenium, antimony, bismuth, and the total amount of
total quantity of mercury, arsenic, selenium, bismuth and antimony
Refers to the measured mercury after the unfiltered sample was digested, arsenic, selenium, bismuth and antimony content.
3.3 analyte
determined elements
Refers to mercury, arsenic, selenium, bismuth and antimony element
4 principle of the method
After the pretreatment of the sample solution into the atomic fluorescence spectrometer, potassium borohydride under acidic conditions (or sodium borohydride) reduction,
Generates arsine, hydrogen bismuth, antimony, hydrogen, hydrogen selenide and mercury atoms, hydrides are formed in an argon atoms in the ground state of hydrogen flame,
Its ground state atom by atom and elemental mercury (mercury, arsenic, selenium, bismuth and antimony) lamp emitted light fluorescence excitation of atoms, atomic fluorescence
Light intensity and content of the analyte in the sample solution within a certain range is proportional.
5 Interference and Elimination
5.1 acidic medium can be reacted with potassium borohydride hydride affect each other interference, anti-thiourea
Ascorbic acid solution (6.20) can substantially eliminate interference.
5.2 above a certain concentration of copper and other transition metals may interfere with the determination, thiourea ascorbic acid solution (6.20),
You can eliminate most of the interference. Under this standard experimental conditions, sample containing Cu2 100 mg/L or less, 50
Fe3, 1 mg mg/L or less Co2/L or less, 10 mg/L or less Pb2 (selenium is 5 mg/L) and 150 mg/L
The following Mn2 (selenium is 2 mg/L) does not affect the determination.
5.3 common anions did not interfere.
5.4 Physical interference cancellation. Selection of two-layer structure of the quartz tube atomizer, the inner and outer layers are argon gas, to form a protective outer layer
Isolated from the air, so that the ground state atoms measured elements do not collide with oxygen and nitrogen in the air, reducing the fluorescence quenching effect on the assay.
6 Reagents and materials
Unless otherwise indicated, analytical chemical reagents used for analysis in line with national standards, test water for the preparation of the new
Deionized or distilled water.
6.1 hydrochloric acid. ρ (HCl) = 1.19 g/ml, pure class distinctions.
6.2 nitric acid. ρ (HNO3) = 1.42 g/ml, pure class distinctions.
6.3 perchloric acid. ρ (HClO4) = 1.68 g/ml, pure class distinctions.
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). pure class distinctions.
6.9 mercuric chloride (HgCl2). pure class distinctions.
6.10 arsenic trioxide (As2O3). pure class distinctions.
6.11 selenium powder. high-purity (mass fraction 99.99%).
6.12 Bismuth. high-purity (mass fraction 99.99%).
6.13 antimony trioxide (Sb2O3). pure class distinctions.
6.14 hydrochloric acid solution. 11.
6.15 hydrochloric acid solution. 595.
6.16 nitric acid solution. 11.
6.17 hydrochloric acid - nitric acid solution
Hydrochloric acid were weighed 300ml (6.1) and 100ml nitrate (6.2), add 400ml water and mix.
6.18 nitric acid - perchloric acid mixture.
With an equal volume of nitric acid (6.2) and perchloric acid (6.3) mixed preparation. When we use the existing service.
6.19 reductant
6.19.1 A solution of potassium borohydride
Weigh 0.5g of sodium hydroxide (6.4) dissolved in 100 ml of water was added 1.0 g of potassium borohydride (6.5), and mix. This solution
The determination of mercury, temporary use when the existing service, stored in a plastic bottle.
6.19.2 potassium borohydride solution B
Weigh 0.5g of sodium hydroxide (6.4) dissolved in 100 ml of water was added 2.0 g of potassium borohydride (6.5), and mix. This solution
In arsenic, selenium, bismuth, antimony determination, temporary use when the existing service, stored in a plastic bottle.
Note. You can also use potassium hydroxide, potassium borohydride reducing agent configuration.
6.20 thiourea - ascorbic acid solution
Each said take 5.0g thiourea (6.6) and ascorbic acid (6.7), with 100 ml of water to dissolve, mixing, measuring preparation day.
6.21 Mercury standard solution
6.21.1 the mercury standard fixative
Weigh 0.5g potassium dichromate (6.8) was dissolved in 950 ml of water, add 50 ml of nitric acid (6.2) and mix.
6.21.2 the mercury standard stock solution. ρ (Hg) = 100mg/L
Purchase a commercially available certified reference materials, or to stand overnight weighed 0.1354g of mercuric chloride (6.9) in a silica gel desiccator
A small amount of mercury standard fixative (6.21.1) dissolved moved 1000ml volumetric flask, dilute with mercury standard fixative (6.21.1) to
Marking, and mix. Store in a glass jar. At 4 ℃ can be stored for 2 years.
6.21.3 mercury intermediate standard solution. ρ (Hg) = 1.00 mg/L
Pipette 5.00ml mercury stock standard solution (6.21.2) in 500ml volumetric flask, add 50ml of hydrochloric acid (6.14), with the mercury standard
Associate fixative (6.21.1) diluted to the mark, and mix. Store in a glass jar. At 4 ℃ can be stored for 100 d.
6.21.4 mercury standard solution. ρ (Hg) = 10.0 μg/L
Pipette 5.00ml amount of mercury intermediate standard solution (6.21.3) in 500ml volumetric flask, add 50ml of hydrochloric acid (6.14), washed with water
Diluted to the mark, and mix. Store in a glass jar. Pro with the existing service.
6.22 Arsenic standard solution
6.22.1 arsenic standard stock solution. ρ (As) = 100 mg/L
Purchase a commercially available certified reference materials, or weighed 0.1320g at 105 ℃ drying 2h superior grade pure arsenic trioxide (6.10) was dissolved
Solutions to 5ml 1mol/L sodium hydroxide solution, with 1mol L hydrochloric acid solution/neutralized to phenolphthalein red faded, moved 1000ml capacity
Bottle diluted with water to the mark, and mix. Store in a glass jar. At 4 ℃ can be stored for 2 years.
6.22.2 arsenic intermediate standard solution. ρ (As) = 1.00mg/L
Pipette 5.00ml arsenic standard stock solution (6.22.1) in 500ml volumetric flask, add 100ml of hydrochloric acid (6.14), washed with water
Diluted to the mark, and mix. At 4 ℃ can be stored for one year.
6.22.3 arsenic standard solution. ρ (As) = 100 μg/L
Pipette 10.00ml arsenic intermediate standard solution (6.22.2) in 100ml volumetric flask, add 20ml of hydrochloric acid (6.14), washed with water
Diluted to the mark, and mix. At 4 ℃ can be stored for 30d.
6.23 selenium standard solution
6.23.1 selenium standard stock solution. ρ (Se) = 100 mg/L
Purchase a commercially available certified reference materials, or weighed 0.1000g powder of high purity selenium (6.11) in 100ml beaker, add 20ml nitric acid
(6.2), low temperature heating and cooling to room temperature, dissolved and transferred to 1000ml volumetric flask, release water to the mark, and mix. Storage
In glass bottles. At 4 ℃ can be stored for 2 years.
6.23.2 selenium intermediate standard solution. ρ (Se) = 1.00 mg/L
Pipette 5.00ml selenium stock standard solution (6.23.1) in 500ml volumetric flask, add 150ml of hydrochloric acid (6.14), washed with water
Diluted to the mark, and mix. At 4 ℃ can be stored for 100 d.
6.23.3 selenium standard solution. ρ (Se) = 10.0 μg/L
Pipette 5.00ml selenium intermediate standard solution (6.23.2) in 500ml volumetric flask, was added 150ml of hydrochloric acid (6.14), washed with water
Diluted to the mark, and mix. Pro with the existing service.
6.24 Bismuth standard solution
6.24.1 bismuth standard stock solution. ρ (Bi) = 100 mg/L
Purchase a commercially available certified reference materials, or weighed 0.1000g high purity metal bismuth (6.12) in 100ml beaker, add 20ml
Nitric acid (6.2), low heat to dissolve completely cooled and transferred to 1000 ml flask, diluted with water to the mark, and mix.
Store in a glass jar. At 4 ℃ can be stored for 2 years.
6.24.2 bismuth intermediate standard solution. ρ (Bi) = 1.00 mg/L
Pipette 5.00ml bismuth stock standard solution (6.24.1) in 500ml volumetric flask, add 100ml of hydrochloric acid (6.14), washed with water
Diluted to the mark, and mix. At 4 ℃ can be stored for one year.
6.24.3 bismuth standard solution. ρ (Bi) = 100 μg/L
Pipette 10.00ml bismuth intermediate standard solution (6.24.2) in 100ml volumetric flask, add 20ml of hydrochloric acid (6.14), washed with water
Diluted to the mark, and mix. Pro with the existing service.
6.25 antimony standard solution
6.25.1 Antimony standard stock solution. ρ (Sb) = 100 mg/L
Purchase a commercially available certified reference materials, or weighed 0.1197g at 105 ℃ drying 2h antimony trioxide (6.13), was dissolved in
80ml hydrochloric acid (6.1), and transferred to 1000ml volumetric flask, then add 120ml of hydrochloric acid (6.1), diluted with water to the mark, mix
uniform. Store in a glass jar. At 4 ℃ can be stored for 2 years.
6.25.2 antimony intermediate standard solution. ρ (Sb) = 1.00 mg/L
Pipette 5.00ml antimony stock standard solution (5.25.1) in 500ml volumetric flask, add 100ml of hydrochloric acid (6.14), washed with water
Diluted to the mark, and mix. At 4 ℃ can be stored for one year.
6.25.3 antimony standard solution. ρ (Sb) = 100 μg/L
Pipette 10.00ml antimony intermediate standard solution (6.25.2) in 100ml volumetric flask, add 20ml of hydrochloric acid (6.14), washed with water
Diluted to the mark, and mix. Pro with the existing service.
6.26 Argon. purity ≥99.999%.
7 instruments and equipment
7.1 atomic fluorescence spectrometer. Instrument performance indicators should be consistent with the provisions of GB/T 21191 of.
7.2 light elements (mercury, arsenic, selenium, bismuth, antimony).
7.3 thermostat heating plate.
7.4 constant temperature water bath. temperature control accuracy of ± 1 ℃.
7.5 filtration device. 0.45 μm pore size microporous membrane River.
7.6 Analytical balance. accuracy of 0.0001g.
7.7 Sample container. glass or rigid polyethylene bottles (barrels).
7.8 commonly used laboratory ware. meet the national standard A-level gauge glass and glassware.
8...