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HJ/T 83-2001 English PDF (HJT83-2001)

HJ/T 83-2001 English PDF (HJT83-2001)

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HJ/T 83-2001: Water quality - Determination of absorbable organic halogen - Ion chromatography method

This Standard specifies ion chromatography method that determines adsorbable organic halogen (AOX) in water.
HJ/T 83-2001
HJ
NATIONAL ENVIRONMENTAL PROTECTION STANDARD
OF THE PEOPLE 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 ??g/L, the concentration range of adsorbable organic fluorine (AOF) is 5~300 ??g/L, and the concentration range of adsorbable organic bromine (AOBr) is 9~1200 ??g/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, ??g/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, ??g/L; 1.866 - the coefficient converted from fluorine to chlorine;
0.444 - the coefficient co...

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