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HJ 669-2013: Water quality. Determination of phosphate. Ion chromatography
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Water quality. Determination of phosphate. Ion chromatography
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HJ 669-2013
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Basic data | Standard ID | HJ 669-2013 (HJ669-2013) | | Description (Translated English) | Water quality. Determination of phosphate. Ion chromatography | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Classification of International Standard | 13.060 | | Word Count Estimation | 10,123 | | Quoted Standard | HJ/T 91; HJ/T 164; HJ 493 | | Regulation (derived from) | Ministry of Environmental Protection Notice No. 63 of 2013 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This standard specifies the determination of water soluble phosphate ion chromatography. This standard applies to the determination of surface water, groundwater and precipitation of soluble phosphate in. Method when the injection volume was 50��l when thi | HJ 669-2013: Water quality. Determination of phosphate. Ion chromatography---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Water quality.Determination of phosphate.Ion chromatography
National Environmental Protection Standard of the People's Republic
Water quality - Determination of phosphate - Ion chromatography
2 0 1 3 - 1 0 - 2 5 released
2 0 1 4 - 0 1 - 0 1 implementation
release
Ministry of Environmental Protection
Content
Foreword. II
1 Scope.1
2 Normative references.1
3 Terms and Definitions 1
4 principle of the method.1
5 interference and elimination 1
6 Reagents and materials 1
7 Instruments and equipment 2
8 sample 2
9 Analysis steps. 2
10 result calculation and representation..3
11 precision and accuracy. 4
12 Quality Control and Quality Assurance 4
13 Notes. 5
Foreword
To implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on Water Pollution Prevention and Control, to protect the environment,
This standard is formulated to ensure human health and to regulate the determination of soluble phosphate in water.
This standard specifies ion chromatography for the determination of soluble phosphate in surface water, groundwater and precipitation.
This standard is the first release.
This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection.
This standard is mainly drafted by. Suzhou Environmental Monitoring Center Station.
This standard is verified by. Suzhou Municipal Center for Disease Control and Prevention, Suzhou Water Supply Company Water Quality Testing Center, China Branch
College Ecological Environment Research Center, Taizhou Environmental Monitoring Center Station, Suzhou Water Environment Monitoring Center and Suzhou Environmental Monitoring
Central station.
This standard was approved by the Ministry of Environmental Protection on October 25,.2013.
This standard has been implemented since January 1,.2014.
This standard is explained by the Ministry of Environmental Protection.
Water quality - Determination of phosphate - Ion chromatography
1 Scope of application
This standard specifies ion chromatography for the determination of soluble phosphate in water.
This standard applies to the determination of soluble phosphate in surface water, groundwater and precipitation.
When the injection volume is 50μl, the detection limit of soluble phosphate (based on PO43-) is 0.007mg/L.
The lower limit of determination is 0.028 mg/L.
2 Normative references
The contents of this standard refer to the following documents or their terms. For undated references, the valid version applies.
In this standard.
HJ/T 91 Surface Water and Wastewater Monitoring Technical Specifications
HJ/T 164 Technical Specifications for Groundwater Environmental Monitoring
HJ 493 Technical regulations for the preservation and management of water sampling samples
3 Terms and definitions
The following terms and definitions apply to this standard.
Soluble ortho-phosphate
Refers to orthophosphoric acid detected by PO43-formation under the chromatographic conditions specified in this standard by filtration through a 0.45 μm microporous membrane.
Salt (including H2PO4-, HPO42- and PO43-).
4 Principle of the method
The orthophosphate in various forms in the sample enters the anion column with a strong alkaline eluent to phosphate (PO43-)
After the form is separated, it is detected by a conductivity detector. According to the retention time qualitative, the external standard method is quantitative.
5 interference and elimination
Certain metal ions may affect the determination of phosphate and may be removed using a cation exchange column (H type); organic in the sample
When the content is high, the C18 column (7.2) is required to remove the interfering substances.
6 reagents and materials
Analytically pure reagents and conductivity less than 0.5 μS/cm were used in the analysis and unless otherwise stated.
0.45 μm microporous membrane filtered deionized water or water of equivalent purity.
6.1 Potassium hydroxide (KOH). excellent grade pure.
6.2 Potassium dihydrogen phosphate (KH2PO4). excellent grade pure.
Bake at 105 ± 5 ° C to constant weight and store in a desiccator.
6.3 Methanol (CH3OH).
6.4 Potassium hydroxide solution. c (KOH) = 100 mmol/L
Weigh 5.610g potassium hydroxide (6.1) dissolved in an appropriate amount of water, dissolved and transferred to a 1000ml volumetric flask, diluted with water to the standard
Line, mix. The solution is a stock solution of the eluent and stored in a polyethylene bottle.
6.5 Potassium dihydrogen phosphate standard stock solution. ρ(PO43-)=1000mg/L
Weigh 1.4329g potassium dihydrogen phosphate (6.2) dissolved in an appropriate amount of water, dissolved and transferred to a 1000ml volumetric flask, diluted with water to
Mark the line and mix. The solution was stored in a polyethylene bottle and stored at 4 ° C for 6 months. You can also buy a commercially available certified standard
liquid.
6.6 Potassium dihydrogen phosphate standard use solution. ρ(PO43-)=10.0mg/L
Accurately measure 1.00ml of potassium dihydrogen phosphate standard stock solution (6.5) in a 100ml volumetric flask, dilute with water to the mark, mix
uniform. The solution can be stored for three months at 4 °C.
6.7 Acetate microporous membrane. 0.45μm pore size (can be used with a syringe).
7 Instruments and equipment
7.1 Ion Chromatograph. An analytical system consisting of an ion chromatograph, operating software, and required accessories.
7.1.1 Column. anion separation column and anion protection column (high capacity alkanol quaternary amine group anion exchange column).
7.1.2 Eluent controller (eluent line generator).
7.1.3 Anion suppressor.
7.1.4 Conductivity detector.
7.2 Pretreatment column. cation exchange column (H-column), C18 solid phase extraction column.
7.3 Syringe. 5ml, 20ml.
7.4 Common instruments and equipment used in general laboratories.
8 samples
8.1 Collection and preservation of water samples
Sample collection was performed in accordance with the relevant regulations of HJ/T 91, HJ/T 164 and HJ 493.
The sample should be filtered through a 0.45 μm microporous membrane. The filtrate is collected in a polyethylene or glass bottle without any preservative.
It can be stored for 48h at 0°C~4°C.
8.2 Preparation of samples
The sample is clean and there is no water sample that interferes with heavy metals or organic matter. After on-site filtration (8.1), it can be directly injected.
Note 1. For samples of unknown concentration, the sample should be diluted 100 times before analysis, and then the appropriate dilution factor should be selected according to the results obtained.
Sample analysis.
Note 2. Samples with heavy metal interference are removed by on-site filtration using a cation exchange column (7.2).
9 Analysis steps
9.1 Instrument Reference Conditions
Operate the instrument according to the instrument manual. Gradient elution reference conditions, see Table 1.
Table 1 Gradient elution reference conditions
t(min) COH-(mmol/L)
0~7 10
7~15 10~40
15~18.5 40
18.5~24 10
Note 3. Eluent flow rate. 1.0ml/min,)
9.2 Calibration
9.2.1 Preparation of the standard series
Accurately measure 0.00ml, 0.20ml, 1.00ml, 2.00ml, 5.00ml, 10.00ml and 20.00ml potassium dihydrogen phosphate respectively
Standard use solution (6.6), dilute to 100 ml with water and mix. Phosphate concentration in the standard series (based on PO43-)
Others. 0.000 mg/L, 0.020 mg/L, 0.100 mg/L, 0.200 mg/L, 0.500 mg/L, 1.00 mg/L, and 2.00 mg/L.
9.2.2 Drawing of the calibration curve
The above standard series were separately filtered through a microporous membrane (6.7), and injected sequentially from low to high concentration, the injection volume was 50 μl.
Chromatograms of different concentrations of phosphate were obtained. The concentration of phosphate (in terms of PO43-, mg/L) is plotted on the abscissa, peak height or peak
The product is plotted on the ordinate and a calibration curve is drawn. The chromatogram of the phosphate ion is shown in Figure 1.
Figure 1 Phosphate ion chromatogram
9.3 Determination
The samples were measured according to the same chromatographic conditions and procedures as those used to draw the calibration curve.
9.4 Blank test
Replace the sample with experimental water and perform a blank test in accordance with step 9.3.
10 Calculation and representation of results
10.1 Calculation of results
The concentration of phosphate in the sample (in terms of PO43-, mg/L) was calculated according to the formula (1).
ρ= f
Ahh ×−− 0 (1)
In the formula.
Ρ--the concentration of phosphate in the sample, mg/L;
H--the peak height (or peak area) of the phosphate in the sample;
H0--the peak height (or peak area) of the phosphate in the blank sample;
B--the slope of the regression equation;
A--the intercept of the regression equation;
F--dilution factor.
10.2 Results are expressed
When the sample content is less than 1mg/L, the result is retained to three decimal places; when the sample content is greater than or equal to 1mg/L,
Keep three significant digits.
11 Precision and accuracy
11.1 Precision
Six laboratories performed uniform samples with phosphate concentrations of 0.033 mg/L, 0.923 mg/L, and 2.137 mg/L, respectively.
The relative standard deviations in the laboratory were 1.7% to 6.6%, 1.3% to 2.8%, and 0.5% to 2.7%, respectively.
The standard deviations were 5.0%, 1.2% and 1.8%, respectively, and the repeatability limits were. 0.004 mg/L, 0.058 mg/L and 0.087 mg/L, respectively.
Reproducibility limits were. 0.006 mg/L, 0.061 mg/L and 0.133 mg/L, respectively.
11.2 Accuracy
6 laboratory-certified reference materials with phosphate concentrations of 0.697 mg/L ± 0.040 mg/L and 0.301 mg/L ± 0.016 mg/L
For the measurement, the relative errors were 0.2% to 3.9% and 0.4% to 2.7%, respectively. The relative error final values are 0.51% ± 0.32% and
1.35% ± 0.90%.
Phosphate concentrations in the six laboratories ranged from 0.012 mg/L to 0.344 mg/L, 0.034 mg/L to 0.595 mg/L, and 0.073 mg/L.
The three actual samples of ~1.14mg/L were spiked and recovered. The recoveries were 94.0% ~103%, 93.0%~102%.
And 97.0%~105%; the final recoveries were 97.2%±3.1%, 97.3%±3.9% and 99.4%±5.2%, respectively.
12 Quality Control and Quality Assurance
12.1 Blank test
At least 2 full program blanks shall be made for each batch of samples, and the blank value shall not exceed the method detection limit. Otherwise, you should find the reason and re
The sample can only be determined after analysis until it is qualified.
12.2 Relevance test
The correlation coefficient of the calibration curve is r ≥ 0.995.
12.3 Intermediate concentration check
For each sample of 20 samples or one batch (less than 20 samples), the concentration of the middle point of a calibration curve should be analyzed.
For the standard solution, the relative error between the measurement result and the concentration of the point at the most recent calibration curve should be ≤10%. Otherwise, you need to redraw
Calibration curve.
12.4 Precision Control
At least 10% of the parallel samples should be determined for each batch of samples. When the number of samples is less than 10, at least one parallel double sample should be determined. when
When the phosphate concentration of the sample is 0.028~0.280mg/L, the relative deviation of the parallel determination results should be ≤20%; when the sample is phosphoric acid
When the salt concentration is 0.280~2.00mg/L, the relative deviation of the parallel determination results should be ≤10%.
12.5 Accuracy Control
At least 10% of the spiked sample shall be determined for each batch of samples. When the number of samples is less than 10, at least one spiked sample shall be determined.
When the phosphate concentration in the sample is 0.028~0.280mg/L, the spike recovery should be between 75~125%; when the sample is phosphate
When the concentration is 0.280~2.00mg/L, the recovery rate of spiked standard should be between 85~115%.
13 Precautions
13.1 Note that the entire system should not enter the bubble, otherwise it will affect the separation effect.
13.2 C18 column should be activated with methanol (6.3) and deionized water before use.
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