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Water quality - Determination of absorbable organic halogen - Ion chromatography method
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HJ/T 83-2001: PDF in English (HJT 83-2001) HJ/T 83-2001
HJ
NATIONAL ENVIRONMENTAL PROTECTION STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
Water quality - Determination of adsorbable
organic halogen - Ion chromatography method
ISSUED ON. DECEMBER 19, 2001
IMPLEMENTED ON. APRIL 01, 2002
Issued by. General Administration of Environmental Protection
Table of Contents
Foreword ... 3
1 Subject content and scope ... 4
2 Definitions ... 4
3 Method and principle ... 5
4 Reagents and materials ... 5
5 Apparatuses and instruments ... 7
6 Sample collection and preservation ... 9
7 Analysis steps ... 9
8 Calculation and result expression ... 12
9 Method precision and accuracy ... 14
10 Description ... 14
Appendix A ... 16
Appendix B ... 17
Foreword
The pre-treatment method (place the activated carbon absorbed with organics in high
temperature furnace to burn, decompose, and transfer into inorganic halides) of water
sample specified in this Standard is basically the same as ISO 9562.1989-09-01 and
GB/T 15959-1995 “Water quality - Determination of adsorbable organic halogens
(AOX) - Microcoulometric method”, however, the detecting methods are different. This
Standard specifies that using ion chromatography method to detect inorganic halogen
ion that is produced and transferred from organic halogen. It can determine not only
the total (in chlorine) of adsorbable organic halogens (AOX) in water, but also the
adsorbable organic chlorine (AOCl), adsorbable organic fluorine (AOF) and
adsorbable organic bromine (AOBr) in water.
Appendix A and appendix B in this Standard are normative.
This Standard shall be under the jurisdiction of General Administration of
Environmental Protection - Science, Technology and Standard Division.
Drafting organization of this Standard. Shenyang Environmental Monitoring Center
Station.
This Standard is first-time released, and it shall be implemented from April 1, 2002.
This Standard shall be interpreted by General Administration of Environmental
Protection.
Water quality - Determination of adsorbable organic
halogen (AOX) - Ion chromatography method
1 Subject content and scope
1.1 Subject content
This Standard specifies ion chromatography method that determines adsorbable
organic halogen (AOX) in water.
1.2 Scope
This Standard applies to determine adsorbable organic halogen (AOX) in water and
polluted water, including adsorbable organic chlorine (AOCl), adsorbable organic
fluorine (AOF) and adsorbable organic bromine (AOBr).
When sample volume is between 50 and 200 ml, it can determine that the
concentration range of adsorbable organic chlorine (AOCl) is 15~600 µg/L, the
concentration range of adsorbable organic fluorine (AOF) is 5~300 µg/L, and the
concentration range of adsorbable organic bromine (AOBr) is 9~1200 µg/L.
1.3 Interference and elimination
1.3.1 Inorganic halogen ion in water, during the sample enrichment process, also can
partly remain in activated carbon to interfere the determination. Use 20 ml of washing
liquid of acidic sodium nitrate (4.12) to leach the activated carbon adsorption column,
so that the interference can be eliminated entirely.
1.3.2 When there are insoluble chloride and biological cells (such as microorganism
and alga) etc. in the water sample, the determination result will be higher; use nitrate
(4.9) to adjust the pH value to be within 1.5~2.0; analyze it after 8 h.
1.3.3 When there is active chlorine in the water sample, the determination result of
AOCl will be higher. Add 5 ml of sodium sulfite solution (4.8) immediately in 100 ml of
water sample, after sampling.
2 Definitions
2.1 adsorbable organic halogen (AOX)
It refers to the total (calculated by Cl) of halogen elements (including fluorine, chlorine
and bromine) which can be adsorbed by activated carbon and can be combined on the
organic compound, under the conditions specified by this Standard.
2.2 adsorbable organic chlorine (AOCl)
It refers to the total of chlorine which can be adsorbed by activated carbon and can be
combined on the organic compound, under the conditions specified by this Standard.
2.3 adsorbable organic fluorine (AOF)
It refers to the total of fluorine which can be adsorbed by activated carbon and can be
combined on the organic compound, under the conditions specified by this Standard.
2.4 adsorbable organic bromine (AOBr)
It refers to the total of bromine which can be adsorbed by activated carbon and can be
combined on the organic compound, under the conditions specified by this Standard.
3 Method and principle
Use activated carbon to adsorb the organic halogen compounds in water; place the
active carbon that have adsorbed organics into high temperature furnace to burn,
decompose, and transfer into hydrogen halide (hydride of fluorine, chlorine and
bromine); use ion chromatography method to separate and determine, after absorbed
by alkaline solution.
4 Reagents and materials
Unless otherwise stated, when analyzing, distilled water free from organics and
analytically pure reagents complying with national standards shall be used.
4.1 distilled water free from organics. use glass distiller to distill deionized water that
has been filtered by activated carbon (4.2) column; distill it before using.
4.2 Activated carbon. analytically pure, 20~60 meshes.
4.3 Purified activated carbon for adsorption use (appendix A).
4.4 Oxygen (O2). 99.9% (V/V).
4.5 5% potassium permanganate solution (m/V).
4.6 10% sodium hydroxide solution (m/V).
4.7 High-purity nitrogen (N2). 99.99% (V/V).
4.8 Sodium sulfite solution, c (Na2SO3)=0.2 mol/L.
7.2.2.1 Adsorption
According to 5.4.1, stuff the activated carbon adsorption column; connect the
adsorption device; take 25~200 ml of preheated water sample (6) according to the
organic contents in the samples; add 5 ml of sodium nitrate stock solution (4.11) in
every 100 ml of water sample; at this moment, the pH value of water sample shall be
less than 2. Otherwise, add nitrate (4.9) to adjust. Move water sample to sample tube
of adsorption device; plug a cover for sealing; adjust nitrogen pressure to let the water
sample to flow past the adsorption column at the speed of 2~3 ml/min. Add 20 ml of
washing liquid of sodium nitrate (4.12) at the speed of 2~3 ml/min to wash the
adsorption column. Also, simple adsorption device (5.4.2) can be used instead of
above steps.
7.2.2.2 Combustion
Preheat up the burner and maintain the temperature at 950±10°C.
Adjust the oxygen pressure and flowmeter to make the speed of blowing oxygen
toward the combustion tube’s inner tube to be 120~150 ml/min, and the speed toward
outer tube be 40~60 ml/min.
Connect the gas-bubble absorption tube (5.6) that contains 3.00 ml of borax
absorbing liquid (4.19) to the outlet of combustion tube; use the asbestos cloth to
wrap the junction to avoid moisture condensation.
Open the silica gel plug at the sample-inlet of combustion tube; use flattened pinhead
(5.9) to move the wet activated carbon that has adsorbed sample in the activated
carbon adsorption column to alumina boat, then plug it.
Push the alumina boat to the preheated zone (furnace’s mouth) of combustion tube;
stay for 2 min; push the alumina boat slowly to the high temperature zone; after 3 min,
pull it out to the sample-inlet. Continue to blow oxygen for 4~5 min.
7.2.2.3 Measurement
Take down the absorption tube and connecting tube from combustion system; use
rubber pipette bulb to blow oxygen from the outlet of absorption tube (Note. do not
blow out the absorbing liquid from bottle), and wash repeatedly to let the fog-drops at
absorption tube’s inlet and in connecting tube to enter into the absorption tube.
Use ion chromatograph to measure the contents of Cl¯, F¯ and Br¯ in the absorption
tube.
7.3 Determination of full-procedure blank samples
Use distilled water to replace the sample; conduct the full-procedure blank test
according to the steps same as that of sample determination.
curve, mg/L.
8.3 Concentration calculation of adsorbable organic bromine (AOBr) in water.
)(
)(
DVCCc BrBrAOBr
Where.
)( AOBrc - the concentration of adsorbable organic bromine (AOBr) in water, µg/L;
Brc - Br¯ concentration in the sample that is found from the standard curve, mg/L;
Brc0 - Br¯ concentration in the blank sample (7.3) that is found from the standard
curve, mg/L.
8.4 Concentration calculation of adsorbable organic halogen (AOX) in water.
)()()()( 444.0866.1 AOBrAOFAOClAOX cccc
Where.
)( AOXc - the concentration of adsorbable organic halogen (AOX) in water, µg/L;
1.866 - the coefficient converted from fluorine to chlorine;
0.444 - the coefficient co...
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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