HJ 535-2009 PDF in English
HJ 535-2009 (HJ535-2009) PDF English
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Water quality. Determination of ammonia nitrogen. Nesslerreagent spectrophotometry
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Standards related to (historical): HJ 535-2009
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HJ 535-2009: PDF in English HJ 535-2009
HJ
NATIONAL ENVIRONMENTAL PROTECTION STANDARD
OF THE PEOPLE’S REPUBLIC OF CHINA
Replacing GB 7479-87
Water Quality – Determination of Ammonia Nitrogen –
Nessler’s Reagent Spectrophotometry
ISSUED ON. DECEMBER 31, 2009
IMPLEMENTED ON. APRIL 1, 2010
Issued by. Ministry of Environmental Protection
Ministry of Environmental Protection of the PRC
Announcement
2009 No.77
To implement Environmental Protection Law of the People’s Republic of China,
protect environment and safeguard the human health, now Air and Exhaust Gas -
Determination of Ammonia - Nessler’s Reagent Spectrophotometry and other four
standards are approved to be national environmental protection standards, and are
published.
Name and number of the standards are as follows.
I. Air and Exhaust Gas - Determination of Ammonia - Nessler’s Reagent
Spectrophotometry (HJ 533-2009);
II. Ambient Air - Determination of Ammonia - Sodium Hypochlorite - Salicylic Acid
Spectrophotometry (HJ 534-2009);
III. Water Quality - Determination of Ammonia Nitrogen – Nessler’s Reagent
Spectrophotometry (HJ 535-2009);
IV. Water Quality - Determination of Ammonia Nitrogen - Salicylic Acid
Spectrophotometry (HJ 536-2009);
V. Water Quality - Determination of Ammonia Nitrogen -
Distillation-Neutralization Titration (HJ 537-2009).
The above standards were implemented since April 1, 2010, published by China
Environmental Science Press; the contents of the standards can be checked at the
website of the Ministry of Environmental Protection (bz.mep.gov.cn).
Since the implementation date of the above standards, the following five published
national environmental protection standards that were approved by the original State
Environmental Protection Agency shall be abolished; the name and number of the
standards are as follows.
I. Air Quality - Determination of Ammonia - Nessler's Reagent Colorimetric Method
(GB/T 14668-93);
II. Air Quality - Determination of Ammonia - Sodium Hypochlorite - Salicylic Acid
Spectrophotometry (GB/T 14679-93);
III. Water Quality - Determination of Ammonium - Nessler's Reagent Colorimetric
Table of Contents
Foreword ... 5
1 Scope ... 7
2 Method Principles ... 7
3 Interference and Elimination ... 7
4 Reagents and Materials ... 8
5 Apparatus and Equipment ... 10
6 Samples ... 10
7 Analysis Procedures ... 11
8 Result Calculation ... 12
9 Accuracy and Precision ... 13
10 Quality Assurance & Quality Control ... 13
Foreword
This Standard was prepared for the purposes of implementing Environmental
Protection Law of the People’s Republic of China, and Water Pollution Prevention and
Control Law of the People's Republic of China, protecting environment, safeguarding
human health, as well as regulating the detection method of ammonia nitrogen in
water.
This Standard specified Nessler’s Reagent Spectrophotometry to measure the
ammonia nitrogen in water.
This Standard revised Water Quality - Determination of Ammonium - Nessler's
Reagent Colorimetric Method (GB 7479-87).
This Standard was first-time published in 1987; the drafting organization of the original
standard was Jiangsu Environmental Monitoring Central Station; this is the first-time
revision. The major revised contents are as follows.
--- Standard name was changed FROM Water Quality - Determination of
Ammonium - Nessler's Reagent Colorimetric Method TO Water Quality -
Determination of Ammonia Nitrogen – Nessler’s Reagent Spectrophotometry.
--- Add the cuvette’s optical path length (10-20mm); reduce the detection limit of
the method; expand the applicable scope of the method. Clearly define the
upper and lower detection limit of the method.
--- Delete the visual colorimetry.
--- Regulate and adjust the structure and format of the standard text.
--- Add the precautions to the key steps such as main reagent preparation and the
sample pretreatment.
--- Combine the calculation formula of the results.
Since the implementation date of this Standard, the Water Quality - Determination of
Ammonium - Nessler's Reagent Colorimetric Method (GB 7479087) that was
approved & published by the original State Environmental Protection Agency on
March 14, 1987 shall be abolished.
This Standard was organized-formulated by Science, Technology and Standard
Division of Ministry of Environmental Protection, Department.
Chief drafting organization of this Standard. Shenyang Environmental Monitoring
Center.
This Standard was approved by Ministry of Environmental Protection on December 31,
Water Quality – Determination of Ammonia Nitrogen –
Nessler’s Reagent Spectrophotometry
Warning. Mercuric chloride (HgCl2) and mercuric iodide (HgI2) are highly toxic
substances; avoid the dermal and oral exposure.
1 Scope
This Standard specifies Nessler’s reagent spectrophotometry to determine the
ammonia nitrogen in water.
This Standard is applicable to determine the ammonia nitrogen in surface water,
underground water, domestic sewage, and industrial waste water.
When the volume of water sample is 50ml, and 20mm cuvette is used; the detection
limit for this method is 0.025mg/L, the lower determination limit is 0.10mg/L, and the
upper determination limit is 2.0mg/L (calculated as per N).
2 Method Principles
Ammonia nitrogen, existed in the free state of ammonia and ammonium ions, reacts
with Nessler’s reagent, and generates light reddish brown complex compound; the
absorbance of such complex compound is proportional to the ammonia nitrogen
contents, then determine the absorbance at the wavelength of 420nm.
3 Interference and Elimination
When water sample contains suspended solids, residual chlorine, metal ions such as
calcium-magnesium, sulfides and organic substances, then they may generate
interference and needs proper treatment, so as to eliminate the influence on the
determination.
If there is residual chlorine in the sample, add proper amount of sodium thiosulfate
solution to remove; use potassium iodide-starch test paper to test whether the
residual chlorine was eliminated completely. When colorization, add proper amount of
potassium sodium tartrate solution, which can eliminate the interference from metal
ions such as calcium-magnesium. If the sample is thick or colorful, it can be treated
with pre-distillation or flocculation methods.
Weigh 20g of hydrochloric acid; dissolve into water; dilute to 1L.
4.12 Bromthymol blue indicator, ρ=0.5g/L.
Weigh 0.05g of bbromthymol blue; dissolve into 50ml of water; add 10ml of anhydrous
ethanol; then use water to dilute to 100ml.
4.13 Potassium iodide-starch test paper
Weigh 1.5g of soluble starch into a beaker; use small amount of water to make it into
paste state; add 200ml of boiling water; stir-mix evenly, and cool down. Add 0.50g of
potassium iodide (KI) and 0.50 g of sodium carbonate (Na2CO3); use water to dilute to
250ml. After immersion of the filter paper, take it out and get dry; then seal-store in the
brown bottle.
4.14 Ammonia nitrogen standard solution
4.14.1 Standard stock solution of ammonia nitrogen, ρN=1000µg/ml.
Weigh 3.8190g of ammonium chloride (NH4Cl, guaranteed reagent, dry for 2h at
100~105°C); dissolve into water; move to 1000ml flask; dilute to the marked-scale; it
can be stored for 1 month at 2~5°C.
4.14.2 Ammonia nitrogen standard working solution, ρN=10µg/ml.
Absorb 5.00ml of ammonia nitrogen standard stock solution (4.14.1) into a 500ml
flask; dilute to the marked-scale. It shall be prepared before use.
5 Apparatus and Equipment
5.1 Visible-light spectrophotometer. with 20mm cuvette.
5.2 Ammonia nitrogen distillation device. consists of 500ml Kjeldahl flask, nitrogen
ball, straight condenser and catheter; the end of condenser can be directly connected
with certain length of dropper, so that the outlet tip is immersed under the absorption
liquid surface. 500ml distillation flask can also be used.
6 Samples
6.1 Sample collection and preservation
Collect water sample into the polyethylene or glass bottle; analyze as soon as
possible. If it needs preserving, add sulfuric acid so as to ; make the acidify the water
sample till pH< 2; it can be stored for 7d at 2~5°C.
9 Accuracy and Precision
For the standard solution of which the ammonia nitrogen concentration is
1.21mg/L, the repeatability limit is 0.028mg/L, the reproducibility limit is 0.075mg/L,
and the recovery rate is 94%~104%.
For the standard solution of which the ammonia nitrogen concentration is
1.47mg/L, the repeatability limit is 0.024mg/L, the reproducibility limit is 0.066mg/L,
and the recovery rate is 95%~105%.
10 Quality Assurance & Quality Control
10.1 The absorbance of reagent blank shall not exceed 0.030 (10mm cuvette).
10.2 Preparation of Nessler’s reagent
In order to guarantee the good color developing ability of the Nessler’s reagent,
during the preparing period, it must control the adding amount of HgCl2, till...
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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