HJ 550-2015_English: PDF (HJ550-2015)
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Water quality. Determination of cobalt. 5-Cl-PADAB Spectrophotometry
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HJ 550-2015
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Standards related to: HJ 550-2015
| Standard ID | HJ 550-2015 (HJ550-2015) | | Description (Translated English) | Water quality. Determination of cobalt. 5-Cl-PADAB Spectrophotometry | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Classification of International Standard | 13.060 | | Word Count Estimation | 9,920 | | Date of Issue | 2015-04-03 | | Date of Implementation | 2015-07-01 | | Older Standard (superseded by this standard) | HJ 550-2009 | | Quoted Standard | HJ/T 91 | | Drafting Organization | Beijing Municipal Environmental Protection Monitoring Center | | Administrative Organization | Ministry of Environment Protection | | Regulation (derived from) | Ministry of Environmental Protection Announcement 2015 No. 20 | | Issuing agency(ies) | Ministry of Environmental Protection | | Summary | This Standard specifies the determination of total dissolved cobalt and cobalt-state 5-chloro-2- (pyridyl) -1, 3-diaminobenzene spectrophotometry. This Standard applies to surface water, industrial wastewater and domestic sewage determination of cobalt. When the sample volume is 20.0ml, method detection limit of 0.009 mg/L, detection limit of 0.036mg/L, measured upper limit is 0.500mg/L. | HJ 550-2015
Water quality.Determination of cobalt.5-Cl-PADAB Spectrophotometry
National Environmental Protection Standard of the People 's Republic of China
Replacing HJ 550-2009
Determination of water quality Cobalt 5-chloro-2- (pyridylazo)
-1,3-diaminobenzene spectrophotometry
Water quality-Determination of cobalt
-5-Cl-PADAB Spectrophotometry
2015-04-03 released
2015-07-01 implementation
Ministry of Environmental Protection released
I directory
Preface II
1 Scope of application
2 normative reference documents
3 Terms and definitions 1
4 Principle of the method
5 interference and elimination
6 reagents and materials 2
7 instruments and equipment 3
8 Sample 3
9 Analysis steps
The results are calculated and expressed
11 Precision and Accuracy
12 Quality assurance and quality control
13 Waste treatment .5
Preface
In order to implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on the Prevention and Control of Water Pollution,
Protect the human health, regulate the monitoring method of cobalt in water, the development of this standard.
This standard is a measure of the determination of total cobalt by 5-chloro-2- (pyridylazo) -1,3-diaminobenzene spectrophotometry (provisional)
(HJ 550-2009).
This standard was first published in.2009, this time for the first revision, this revision mainly on the scope of application of the method,
Methodology, Interference and Elimination, Reagents and Materials, Instruments, Samples, Analytical Steps, Results Calculations and Representations, Precision
Degree and accuracy of the contents of the re-provided. Added normative references to documents, terms and definitions, quality assurance and quality
Control and so on.
From the date of implementation of this standard, "Determination of total cobalt water 5-chloro-2- (pyridylazo) -1,3-diaminobenzene spectrophotometry
(Provisional) "(HJ 550-2009).
This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division.
The drafting of this standard. Beijing Environmental Protection Monitoring Center.
The standard verification unit. Chaoyang District, Beijing Environmental Protection Monitoring Station, Yanqing County Environmental Protection Monitoring Station, Tsinghua University Ring
Environmental quality testing center, Beijing Kangju environmental testing station, Beijing China measured North Detection Technology Co., Ltd., Beijing Environmental Protection
Monitoring center.
This standard is approved by the Ministry of Environmental Protection on April 03,.2015.
This standard has been implemented since July 1,.2015.
This standard is explained by the Ministry of Environmental Protection.
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Determination of water quality Cobalt 5-chloro-2- (pyridylazo)
1,3-diaminobenzene spectrophotometry
1 Scope of application
This standard specifies the determination of dissolved cobalt and total cobalt in water 5-chloro-2- (pyridylazo) -1,3-diaminobenzene spectrophotometry
law.
This standard applies to the determination of cobalt in surface water, industrial waste water and domestic sewage.
When the sampling volume of 20.0ml, the detection limit of 0.009mg/L, the determination of the lower limit of 0.036mg/L, determination of the upper limit
Is 0.500mg/L.
2 normative reference documents
The contents of this standard refer to the terms of the following documents. For those who do not mind the date of the reference file, the valid version applies
In this standard.
Technical specification for surface water and wastewater monitoring
3 terms and definitions
The following terms and definitions apply to this standard.
3.1 dissolved cobalt
Refers to cobalt that has not been acidified after passing through a 0.45 μm pore size filter.
3.2 Total Cobalt
Refers to the sum of the cobalt in two parts of the dissolved and suspended phases of the sample, as measured by the unfiltered sample.
4 principle of the method
Cobalt is reacted with 5-chloro-2- (pyridylazo) -1,3-diaminobenzene (5-Cl-PADAB) to form a magenta complex.
570nm wavelength measured its absorbance, absorbance and cobalt concentration in line with the law of Lang Beibei.
5 interference and elimination
5.1 In 25ml color system, when a single ion interference exists, Fe2 content greater than 0.1mg when there is negative interference, Cr3
Content of more than 0.5μg when there is positive interference, Cr6 content of more than 2μg when there is negative interference, Cu2 content of more than 0.5μg when the negative dry
Disturb. After digestion of the sample, 0.5 ml of sodium pyrophosphate (6.12) was added to remove 0.3 mg of Fe2 interference, 1.5 g of dry
Interference, 4μgCr6 interference, 1.5μgCu2 interference.
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5.2 in 25ml color system, Fe3 content of more than 4μg above the positive interference. In the pH = 5 ~ 6 conditions, add the appropriate amount
Sodium pyrophosphate solution to iron brown disappeared, then add 2.5ml sodium pyrophosphate (6.12), can remove 6μgFe3 interference.
5.3 Al3, Cd2, Zn2, Mg2, Ca2, Ni2, SO42-, Cl-, PO43-, NO3-, Br-, ClO4-
Determination.
6 reagents and materials
Unless otherwise stated, analytical reagents conforming to national standards are used for analysis. Experimental water is a newly prepared deionized
Water or distilled water.
6.1 nitric acid. ρ (HNO3) = 1.42g/ml, excellent grade pure.
6.2 perchloric acid. ρ (HClO4) = 1.67g/ml, excellent grade pure.
6.3 Hydrochloric acid. ρ (HCl) = 1.19g/ml, excellent grade pure.
6.4 Sulfuric acid. ρ (H2SO4) = 1.84g/ml, excellent grade pure.
6.5% acetic acid.
6.6 95% ethanol.
6.7 hydrochloric acid solution. 1 1.
6.8 Cobalt trioxide. Spectrum pure.
6.9 Sodium hydroxide. ω (NaOH) = 40%.
Weigh 40.0 g of sodium hydroxide and dissolve in 100 ml of water.
6.10 acetic acid - sodium acetate (HAC-NaAC) buffer solution. pH = 5 ~ 6.
Weigh 21.0g anhydrous sodium acetate, dissolved in a small amount of water, add acetic acid to adjust the pH to 5 to 6, diluted with water to 1000ml,
Is now available.
6.11 5-C1-PADAB Ethanol solution. ω (5-C1-PADAB) = 0.05%.
Weigh 0.05g 5-C1-PADAB, dissolved in 100ml 95% ethanol solution, stored in a brown bottle, is now available.
6.12 Sodium pyrophosphate solution. ω (Na4P2O7 · 10H2O) = 5%.
Weigh 5.0g sodium pyrophosphate, dissolved in water, diluted to 100ml, is now available with.
6.13 cobalt standard stock solution. ρ (Co) = 0.100mg/L.
Weigh 0.0703 g of cobalt oxide (6.8), dissolved in 5.0 ml of hydrochloric acid (6.3), transferred to a 500 ml volumetric flask,
Diluted with water to the mark, 4 ℃ can be stored for at least one month. Commercial reference materials may also be used.
6.14 cobalt standard use of liquid. ρ (Co) = 2.00μg/ml.
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Absorb 10.00ml cobalt standard stock solution (6.13), into the 500ml volumetric flask, diluted with water to the mark, now use
With
6.15 p-nitrophenol solution. ω (C6H5NO3) = 0.2%.
Weigh 0.20g p-nitrophenol, dissolved in water, diluted to 100ml, is now available with.
6.16 filter. 0.45μm acetate filter.
7 instruments and equipment
Unless otherwise stated, all Class A glass gauges conforming to national standards are used for analysis.
7.1 Visible Spectrophotometer. A cuvette with an optical path of 20mm.
7.2 thousandth of a balance.
7.3 Laboratory equipment and glassware.
8 samples
8.1 Collection and storage of samples
Collect water samples according to HJ/T 91 surface water and wastewater monitoring technical specifications. After the sample was collected, add sulfuric acid (6.4) or nitric acid (6.1)
To pH < 2, stored at 0 ℃ ~ 4 in cold storage for 14 days.
Note 1. When collecting dissolved cobalt, it should be filtered through a 0.45 μm pore size filter before adding acid.
8.2 Preparation of the sample
The samples were prepared by digestion with nitric acid and perchloric acid.
Absorb water samples 2.00 ~ 20.0ml (depending on the water content of cobalt) in 100ml beaker, add l ~ 2ml nitric acid (6.1),
Cover the surface of the dish, in the heating plate to boil for 1 ~ 5min, remove the slightly cold, add l ~ 2ml perchloric acid (6.2) (depending on organic
Subject matter content), continue to heat to smoke thick smoke, and continued until the solution without black residue transparent so far. Remove the cooling
After adding l ~ 2 drops of p-nitrophenol indicator (6.15), add 40% sodium hydroxide solution (6.9) to the solution to yellow,
The total volume can not exceed 5ml, to be measured.
8.3 Preparation of blank sample
Absorb 2.00 ~ 20.0ml distilled water in 100ml beaker, the following steps with (8.2).
9 Analysis steps
9.1 Drawing of working curves
9.1.1 digestion
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Respectively, the use of cobalt standard solution (6.14) 0.00,0.25,0.50,1.00,1.50,2.00ml in 100ml beaker,
Distilled water was added to about 5 ml and digested with the same step (8.2).
9.1.2 Draw the working curve
The digested standard solution series (9.1.1) was transferred to 25 ml of a plug colorimetric tube,
Distilled water washed 2 to 3 times, the washing liquid into the colorimetric tube, the total volume can not exceed 8ml. 5.0 ml of acetic acid-acetic acid was added
Sodium buffer solution (6.10), 0.50 ml sodium pyrophosphate solution (6.12), 1.00 ml 5-Cl-PADAB solution (6.11)
Shake well Placed in boiling water bath for 5min, remove, add hot 10ml (1 1) hydrochloric acid solution (6.7), with water dilute
Release to the mark, shake. After cooling, the absorbance was measured with a 20 mm cuvette at a wavelength of 570 nm. To
The calibration curve was plotted against the absorbance of the reagent blank.
9.2 Sample analysis
9.2.1 Determine with the digested water sample (8.2), with the drawing of the working curve step (9.1.2).
Note 2. If the water content of trivalent iron is high, should be appropriate to add sodium pyrophosphate solution, drawing the working curve of sodium pyrophosphate solution should be used with the determination
Water samples are the same.
9.2.2 blank sample analysis
The digested blank sample (8.3) was measured with the step (9.1.2) of drawing the working curve.
10 results are calculated and expressed
10.1 Result calculation
The mass concentration of cobalt in the sample is calculated according to equation (1)
BV
Ay
BV
Ay 001 (Co) (1)
Where. ρ (Co) - mass concentration of cobalt in the sample, mg/L;
1 ü - mass concentration of cobalt in the sample from the working curve, mg/L;
0 £ - mass concentration of cobalt in blank samples taken from the working curve, mg/L;
Y - the absorbance value of the test sample;
0y - measure the absorbance of the blank sample;
B - the slope of the working curve;
A - the intercept of the working curve, μg;
V - water sample volume, ml.
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10.2 results are shown
When the measurement result is less than 1 mg/L, the result is retained to three decimal places; when the measurement result is greater than or equal to 1 mg/L
, The result retains three significant digits.
11 precision and accuracy
11.1 precision
Six laboratories carried out uniform standard samples with a concentration of 0.400mg/L, 2.00mg/L and 3.60mg/L respectively
Parallel test. the relative standard deviation in the laboratory were. 0.7% ~ 4.0%, 0.9% ~ 1.4%, 0.3% ~ 1.2%; experiment
The relative standard deviations were 5.3%, 0.4%, 0.3%, and the repeatability r was 0.034 mg/L, 0.070 mg/L, 0.070
Mg/L; reproducibility limit R was 0.068 mg/L, 0.073 mg/L, 0.074 mg/L, respectively.
11.2 Accuracy
6 laboratories were used to determine the concentration of 0.141 ± 0.013mg/L, 1.15 ± 0.08mg/L standard samples were.
The relative errors in the laboratory were -2.1% ~ 3.6%, - 0.9% ~ 1.7%, respectively. The relative errors were 0.5%
0.04%, 0.3% ± 0.03%.
Six laboratories were on the surface water, domestic sewage, industrial wastewater samples were measured by the standard recovery. laboratory
The recoveries were 99.7% ~ 101%, 94.3% ~ 98.6% and 94.7% ~ 106%, respectively.
The values were 99.5% ± 2.0%, 97.3% ± 4.6% and 98.7% ± 8.2%, respectively.
12 quality assurance and quality control
12.1 each batch of samples should be at least a full blank test and laboratory blank test, the determination of the results should be lower than the method
The detection limit.
12.2 The correlation coefficient of the working curve should be ≥0.999.
12.3 per batch of samples should be analyzed calibration curve intermediate point concentration standard solution, the determination of the results and calibration curve of the middle point of concentration
The relative deviation of the degree should be ≤ 10%, otherwise, need to re-draw the calibration curve.
12.4 each batch of samples should be done spike recovery determination, spike recovery rate should be 90% to 110% range.
12.5 Each sample of 10 samples should be tested in parallel, with less than 10 samples, at least once
Parallel sample determination, the two parallel sample analysis results relative deviation should be less than 10%.
13 Waste treatment
During the course of the experiment, the waste liquid should be placed in a suitable container for centralized storage and handled by a qualified unit.
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