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Water Quality - Determination of Water Soluble Cations(Li+, Na+, NH4+, K+, Ca2+, Mg2+) - Ion Chromatography
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Basic data Standard ID | HJ 812-2016 (HJ812-2016) | Description (Translated English) | Water Quality - Determination of Water Soluble Cations(Li+, Na+, NH4+, K+, Ca2+, Mg2+) - Ion Chromatography | Sector / Industry | Environmental Protection Industry Standard | Classification of Chinese Standard | Z16 | Word Count Estimation | 13,185 | Date of Issue | 2016-07-26 | Date of Implementation | 2016-10-01 | Regulation (derived from) | Ministry of Environmental Protection Notice No.52 of 2016 | Issuing agency(ies) | Ministry of Ecology and Environment |
HJ 812-2016: Water Quality - Determination of Water Soluble Cations(Li+, Na+, NH4+, K+, Ca2+, Mg2+) - 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.
(Determination of Water Soluble Cations (Li, Na, NH4, K, Ca2, Mg2) Ion Chromatography)
National Environmental Protection Standard of the People 's Republic of China
2016-07-26 release
2016-10-01 implementation
Ministry of Environmental Protection released
Directory
Preface ii
1 Scope of application
2 normative reference documents
3 Principle of the method
4 interference and elimination
5 reagents and materials
6 instruments and equipment
7 samples .3
8 Analysis steps
The results are calculated and expressed
10 precision and accuracy 5
11 Quality assurance and quality control
12 Waste treatment 6
13 Precautions 6
Appendix A (informative) method of precision and accuracy
Appendix B (informative) Chromatogram of Cationic Standard Solution
Foreword
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,
Barrier to human health, regulate the determination of soluble cations in water, the development of this standard.
This standard specifies the determination of six soluble cations in water (Li, Na, NH4
, K, Ca2, Mg2)
law.
This standard is the first release.
Appendix A and Appendix B of this standard are informative.
This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division.
The drafting unit of this standard. Gansu Province Environmental Monitoring Center Station.
The standard verification unit. Xiamen University School of Chemistry and Chemical Engineering, Guangzhou University Analysis and Testing Center, Gansu Province Jiayuguan City Environmental Protection
Monitoring station, Beijing Physical and Chemical Analysis and Testing Center, Inner Mongolia Hulunbeier City Environmental Monitoring Station, Guangdong Environmental Protection Engineering Vocational
Courtyard and Gansu Province Zhangye City Environmental Monitoring Station.
The environmental protection department of this standard approved on July 26,.2016.
This standard has been implemented since October 1,.2016.
This standard is explained by the Ministry of Environmental Protection.
Water soluble cation (Li, Na, NH4
, Ca2, Mg2) was determined by ion chromatography
1 Scope of application
This standard specifies the determination of soluble cations in water (Li, Na, NH4
, K, Ca2, Mg2)
Spectrum method.
This standard applies to surface water, groundwater, industrial wastewater and domestic sewage in the six kinds of soluble cation (Li, Na,
NH4
, K, Ca2, Mg2).
When the injection volume of 25 μl, the method of 6 kinds of soluble cation method detection limit and determination of the lower limit in Table 1.
Table 1 Method Detection limit and lower limit of determination (mg/L)
Ion name Li Na NH4
K Ca2 Mg2
method
The detection limit
0.01 0.02 0.02 0.02 0.03 0.02
Determination of the lower limit of 0.04 0.08 0.08 0.08 0.12 0.08
2 normative reference documents
The contents of this standard refer to the following documents or their terms. Any annotated file that does not specify the date, its valid version
Applicable to this standard.
Technical Guidance for Water Quality Sampling
Technical specification for surface water and wastewater monitoring
Technical specification for groundwater environmental monitoring
3 Principle of the method
Water samples in the cation, the cationic column exchange separation, inhibition or non-inhibitory conductivity detector detection,
According to the retention time qualitative, peak height or peak area quantification.
4 interference and elimination
4.1 Some of the hydrophobic compounds in the sample may affect the chromatographic separation and column life. RP
Column or C18 column treatment to eliminate or reduce its impact.
4.2 on the retention time similar to the two kinds of cations, when the concentration difference between the larger and low concentration of ions measured,
Excessive dilution, adjust the flow rate, change the eluent ratio, etc. to eliminate or reduce interference.
5 reagents and materials
Unless otherwise stated, analytical reagents conforming to national standards are used for analysis. Experimental water for the resistivity ≥ 18
MΩ · cm (25 ° C) and filtered through a 0.45 μm microporous membrane.
5.1 concentrated nitric acid (HNO3). excellent grade pure, ρ = 1.42 g/ml.
5.2 lithium nitrate (LiNO3). excellent grade, should be used before the 105 ℃ ± 5 ℃ dry constant weight, placed in a dryer to save.
5.3 sodium nitrate (NaNO3). excellent grade pure, should be used before the 105 ℃ ± 5 ℃ dry constant weight, placed in the dryer in the insurance
Save
5.4 ammonium chloride (NH4Cl). excellent grade, should be used before the 105 ℃ ± 5 ℃ dry constant weight, placed in a dryer to save.
5.5 potassium nitrate (KNO3). excellent grade, should be used before the 105 ℃ ± 5 ℃ dry constant weight, placed in a dryer to save.
5.6 calcium nitrate [Ca (NO3) 2 · 4H2O]. excellent grade pure, should be placed in the dryer before the balance 24 h.
5.7 magnesium nitrate [Mg (NO3) 2 · 6H2O]. excellent grade, should be placed in the dryer before use for 24 h.
5.8 Methanesulfonic acid. (CH3SO3H) ≥99%.
5.9 Nitric acid solution. c (HNO3) = 1 mol/L.
Remove 68.26 ml of concentrated nitric acid (5.1) slowly adding water, dilute to 1000 ml with water and mix well.
5.10 Lithium ion standard stock solution. ρ (Li) = 1000 mg/L.
Weigh 9.9337 g of lithium nitrate (5.2) dissolved in the amount of water, the whole volume into the 1000 ml volumetric flask, diluted with water volume
To mark, mix well. Transferred to the polyethylene bottle, in the 4 ℃ below the cold, dark and sealed can be stored for 6 months. Also available for purchase
Buy a commercially available standard material.
5.11 sodium ion standard stock solution. ρ (Na) = 1000 mg/L.
Weigh 3.6977 g sodium nitrate (5.3) dissolved in the amount of water, the whole volume into 1000 ml volumetric flask, diluted with water volume
To mark, mix well. Transferred to the polyethylene bottle, in the 4 ℃ below the cold, dark and sealed can be stored for 6 months. Also available for purchase
Buy a commercially available standard material.
5.12 ammonium ion standard stock solution. ρ (NH4
) = 1000 mg/L.
Weigh 2.9654 g ammonium chloride (5.4) dissolved in the amount of water, the whole volume into the 1000 ml volumetric flask, diluted with water volume
To mark, mix well. Transferred to the polyethylene bottle, in the 4 ℃ below the cold, dark and sealed can be stored for 6 months. Also available for purchase
Buy a commercially available standard material.
5.13 potassium ion standard stock solution. ρ (K) = 1000 mg/L.
Weigh 2.5857 g potassium nitrate (5.5) dissolved in the amount of water, the whole volume into the 1000 ml volumetric flask, diluted with water volume
To mark, mix well. Transferred to the polyethylene bottle, in the 4 ℃ below the cold, dark and sealed can be stored for 6 months. Also available for purchase
Buy a commercially available standard material.
5.14 Calcium ion standard stock solution. ρ (Ca2) = 1000 mg/L.
Weigh 5.8919 g calcium nitrate (5.6) dissolved in the amount of water, the whole volume into the 1000 ml volumetric flask, add 1.00 ml
Nitric acid solution (5.9), diluted with water volume to the mark, mix. Transferred to the polyethylene bottle, at 4 ℃ below the cold, avoid
Light and seal can be stored for 6 months. You can also purchase commercially available certified materials.
5.15 magnesium standard stock solution. ρ (Mg2) = 1000 mg/L.
Weigh 10.5518 g magnesium nitrate (5.7) dissolved in the amount of water, the whole volume into the 1000 ml volumetric flask, add 1.00 ml
Nitric acid solution (5.9), diluted with water volume to the mark, mix. Transferred to the polyethylene bottle, at 4 ℃ below the cold, avoid
Light and seal can be stored for 6 months. You can also purchase commercially available certified materials.
5.16 mixed standard use of liquid
Respectively, 10.0 ml lithium ion standard stock solution (5.10), 250 ml sodium standard solution (5.11), 10.0
Ml ammonium ion standard stock solution (5.12), 50.0 ml potassium ion standard stock solution (5.13), 250 ml calcium ion standard storage
(5.14), 50.0 ml of magnesium ion standard stock solution (5.15) in a 1000 ml volumetric flask, diluted with water to
Marking, mixing. Formulated with 10.0 mg/L of Li, 250 mg/L of Na, 10.0 mg/L of NH4
, 50.0 mg/L
Of K, 250 mg/L of Ca2 and 50.0 mg/L of Mg2 for mixed standard use of the solution.
5.17 eluent
According to the instrument model and column instructions for the use of conditions for preparation. The eluent conditions given below are for reference.
5.17.1 Methanesulfide leaching stock solution. c (CH3SO3H) = 1 mol/L.
Remove 65.58 ml of methanesulfonic acid (5.8) in the appropriate amount of water, the whole volume into the 1000 ml volumetric flask, diluted with water volume
To mark, mix well. The solution is stored in a glass reagent bottle and can be stored at room temperature for 3 months.
5.17.2 Methanesulfonic acid leaching liquid. c (CH3SO3H) = 0.02 mol/L.
Remove 40.00 ml of methanesulfonic acid leachate (5.17.1) in a.2000 ml volumetric flask, dilute to volume with water,
Mix well.
5.17.3 Nitrate leaching using liquid. c (HNO3) = 7.25 mmol/L.
Remove 14.50 ml of nitric acid solution (5.9) in a.2000 ml volumetric flask, dilute with constant volume to the mark, mix well.
6 instruments and equipment
6.1 Ion Chromatograph. An analytical system consisting of an ion chromatograph, operating software, and required accessories.
6.1.1 Column. cation separation column (polydivinylbenzene/ethyl vinyl benzene, with carboxylic acid or phosphoric acid functional group, high
Capacity column) and cation protection column. A sample can be used to determine the six cations specified in this method
Less than 1.5.
6.1.2 Cationic Suppressor (optional).
6.1.3 Conductivity Detector.
6.2 suction filter device. with a pore size ≤ 0.45 μm acetate fiber or polyethylene filter.
6.3 One-time water microporous membrane syringe filter. aperture 0.45 μm.
6.4 Disposable syringes. 1 ml to 10 ml.
6.5 Pretreatment Column. Polystyrene-divinylbenzene as the substrate of the RP column or silica gel for the matrix-bonded C18 column (removal of hydrophobicity
Compounds) and the like.
6.6 Common laboratory equipment and equipment.
7 samples
7.1 Collection and storage of samples
Samples were collected according to the relevant regulations of HJ 494, HJ/T 91 and HJ/T 164. Samples collected should be divided as soon as possible
Analysis. If it can not be measured in time, should be filtered through the filter device (6.2), refrigerated at 4 ° C below, protected from light. different
The storage time and container material requirements of the ions to be measured are shown in Table 2.
Table 2 Water storage conditions and requirements
Cave contains the material storage time of the container
Li polyethylene bottle for 7 days
Na polyethylene bottle for 7 days
NH4
Polyethylene bottles or hard glass bottles for 2 days
K polyethylene bottle for 7 days
Ca2 polyethylene bottle or hard glass bottle for 7 days
Mg2 polyethylene bottle or hard glass bottle for 7 days
7.2 Preparation of the sample
For clean water samples that do not contain interfering substances such as hydrophobic compounds, they are filtered through a suction filter (6.2)
(6.4) with a water-based microporous membrane syringe filter (6.3). On the dry
Disturbance of complex water quality samples, the corresponding pre-treatment column (6.5) for effective removal and then injection.
7.3 Preparation of blank samples
The sample was prepared in the same manner as in the preparation of the sample (7.2).
8 Analysis steps
8.1 Ion chromatographic analysis of the reference conditions
According to the instrument manual to optimize the measurement conditions or parameters, according to the actual sample matrix and composition optimization eluent
concentration. The following conditions are given for the analysis of ion chromatographic conditions.
8.1.1 Reference condition 1
Cation separation column (6.1.1). Methanesulfonic acid leaching using the solution (5.17.2), flow rate. 1.0 ml/min;
Lead detector, continuous self - circulation regenerator. Injection volume. 25 μl. Cationic standard solution chromatography under this reference condition
See Figure B.1 in Appendix B.
8.1.2 Reference conditions 2
Cation separation column (6.1.1). Nitrate leaching using liquid (5.17.3), flow rate. 0.9 ml/min; non-inhibitory power
Lead detector. Injection volume. 25 μl. The chromatogram of the cationic standard solution under this reference is shown in Figure B.2 in Appendix B.
8.2 Standard curve drawing
Respectively, accurate removal of 0.00 ml, 1.00 ml, 2.00 ml, 5.00 ml, 10.0 ml, 20.0 ml mixed standard use of liquid
(5.16) placed in a group of 100 ml volumetric flask, diluted with water volume to the mark, mix. Prepared into 6 different concentrations
Mixed standard series, the standard series of mass concentration in Table 3. According to the concentration of the measured sample to determine the appropriate standard series of concentrated
Degree range. According to their concentration from low to high order in turn into the ion chromatograph, record the peak area (or peak height). To separate
The mass concentration of the child is the abscissa, the peak area (or peak height) is the ordinate, and the standard curve is drawn.
Table 3 Cationic Standard Series Mass Concentration
Ion Name Standard Series Mass Concentration (mg/L)
Li 0.00 0.10 0.20 0.50 1.00 2.00
Na 0.00 2.50 5.00 12.5 25.0 50.0
NH4
0.00 0.10 0.20 0.50 1.00 2.00
K 0.00 0.50 1.00 2.50 5.00 10.0
Ca2 0.00 2.50 5.00 12.5 25.0 50.0
Mg2 0.00 0.50 1.00 2.50 5.00 10.0
8.3 Determination of samples
The sample (7.2) was injected into the ionic color according to the same chromatographic conditions (8.1) and (8.2) as the standard curve
The cationic concentration was measured by a spectrometer to qualify the retention time, and the instrument response was quantified.
Note 1. If the test results exceed the standard curve range, the sample should be diluted with experimental water and then re-measured; can be diluted 50 to
100 times the post-test sample, and then select the appropriate results according to the results of the re-injection of the sample re-injection analysis, while recording the sample dilution factor (f).
8.4 blank test
The blank sample (7.3) was injected into an ion chromatograph according to the same chromatographic conditions and procedures as the test (8.3) of the sample
Determination of cation concentration, to retain the time qualitative, instrument response quantitative.
9 Results calculation and representation
9.1 Results calculation
Soluble cations in the sample (Li, Na, NH4
, K, Ca2, Mg2) mass concentration (, mg/L),
Calculated according to formula (1).
Ahh 0 (1)
Where. - mass concentration of cation in sample, mg/L;
H - the peak area (or peak height) of the cation in the sample;
0h - peak area (or peak height) of the cation in the laboratory blank sample;
A - the intercept of the regression equation;
B - the slope of the regression equation;
F - sample dilution factor.
9.2 The result is shown
When the sample content is less than 1 mg/L, the result is retained to two decimal places; when the sample content is greater than or equal to 1 mg/L
, The result retains three significant digits.
10 precision and accuracy
10.1 Precision
7 laboratories containing Li, Na, NH4
, K, Ca2, Mg2 at different concentrations of uniform samples were measured
The relative standard deviations in the laboratory range from 0.1% to 7.0%; the relative standard deviations in the laboratory range from 0.9%
~ 10.0% between. Method The precision test results are given in Table A.1 in Appendix A.
10.2 Accuracy
Seven laboratories were tested for different types of water samples, and the recoveries were in the range of 83.6%
~ 113.8% between. The accuracy of the method is shown in Table A.2 in Appendix A.
11 quality assurance and quality control
11.1 Blank test
Each batch (≤20) sample should be at least two laboratory blank test, the blank test results should be lower than the method detection limit.
Otherwise, the cause should be identified and the sample can not be measured until it is passed.
11.2 Relevance test
The correlation coefficient of the standard curve should be ≥ 0.995, otherwise the standard curve should be redrawn.
11.3 Continuous calibration
Each batch (≤ 20) samples, should be a standard curve of the concentration of the standard solution, the determination of the results and standard
The relative error between the concentration of the quasi-curve should be ≤10%. Otherwise, the standard curve should be redrawn.
11.4 Precision control
Each batch (≤ 20) samples, should be measured at least 10% of the parallel sample, the number of samples less than 10, should be at least measured
Set a parallel double sample. The relative deviation of the results of the parallel two-phase measurement should be ≤10%.
11.5 Accuracy control
Each batch (≤ 20) samples, should be done at least one spike recovery, the actual sample of the spike recovery rate should be controlled
Between 80% and 120%.
12 Waste treatment
The waste generated in the experiment should be collected collectively, properly kept, commissioned by qualified units.
13 Precautions
13.1 Analysis of wastewater samples, the pretreatment column used should be able to effectively remove the hydrophobic compounds in the sample matrix, while
No adsorption occurs on the measured cations.
13.2 high concentration of heavy metals and transition metal ions, will affect the separation of separation column and service life. Should be used when used
The column was regenerated on a regular basis using a high concentration of eluent and complexing agent, as required by the column brochure.
Appendix A
(Informative)
Method of precision and accuracy
The data on the accuracy and accuracy of the seven laboratories are summarized in Table A.1 and Table A.2.
Table A.1 The precision of the method
ion
name
Precision
average value/
(Mg/L)
Laboratory relative
standard deviation/ %
Inter-laboratory relative
standard deviation/ %
Repeatability limit
R/(mg/L)
Reproducibility limit
R/(mg/L)
Li
0.02 0.5 to 4.9 10.0 0.01 0.01
0.20 0.2 to 1.2 2.7 0.01 0.02
2.00 0.1 to 1.3 1.2 0.04 0.07
Na
0.24 0.4 to 3.8 3.4 0.01 0.03
1.01 0.1 to 7.0 3.0 0.09 0.12
9.95 0.1 to 2.0 0.9 0.27 0.36
NH4
0.13 1.2 to 5.6 8.0 0.01 0.03
1.02 0.2 to 3.6 1.7 0.05 0.07
4.94 0.1 to 1.5 1.7 0.10 0.26
0.12 0.6 to 5.9 5.4 0.01 0.02
1.99 0.1 to 3.5 2.9 0.10 0.19
10.0 0.1 to 1.3 1.9 0.20 0.56
Ca2
0.56 0.3 to 3.6 3.3 0.03 0.06
1.00 0.1 to 2.3 2.9 0.04 0.09
10.0 0.1 to 1.8 1.0 0.26 0.36
Mg2
0.20 0.5 to 4.4 4.9 0.02 0.03
1.01 0.1 to 2.1 1.9 0.09 0.10
10.0 0.1 to 1.4 0.9 0.22 0.33
Table A.2 The accuracy of the method
Ion name sample type
The original concentration /
(Mg/L)
Plus scalar /
(Mg/L)
Spiked recovery rate
Pi /%
The final value of the recoveries
S2 ± /%
Li -
Surface water ND 0.10 86.2 ~ 94.4 91.0 ± 6.2
Groundwater ND 0.10 89.6 ~ 95.3 92.3 ± 4.2
Domestic sewage ND 0.10 89.3 ~ 107.0 96.3 ± 15.0
Industrial Wastewater ND 0.10 92.3 ~ 100.9 95.9 ± 6.8
Na -
Surface water 24.0 10.0 89.1 to 98.4 91.5 ± 9.8
Groundwater 6.07 5.00 99.4 ~ 109.3 103.6 ± 8.6
Domestic sewage 1.77 2.00 93.6 ~ 107.9 98.6 ± 9.6
Industrial Wastewater 1.99 2.00 88.5 ~ 103.5 94.2 ± 10.2
NH4
Surface water ND 2.50 85.9 ~ 94.7 90.8 ± 7.2
Groundwater ND 2.50 87.0 ~ 92.4 90.7 ± 3.8
Domestic sewage 0.16 0.20 84.9 ~ 105.3 97.8 ± 14.0
Industrial Wastewater 0.01 0.50 94.2 ~ 109.1 101.2 ± 11.0
K -
Surface water 1.36 1.50 88.9 to 113.8 99.3 ± 16.8
Groundwater ND 2.50 84.6 ~ 97.4 89.9 ± 8.8
Domestic sewage 0.11 0.20 89.8 ~ 112.0 103.4 ± 14.4
Industrial Wastewater 0.46 0.50 84.4 ~ 106.8 92.9 ± 17.2
Ca2
Surface water 36.0 20.0 98.8 ~ 111.1 103.4 ± 8.6
Groundwater 16.1 10.0 85.2 ~ 90.1 87.8 ± 3.4
Domestic sewage 0.77 1.00 90.7 ~ 109.0 98.4 ± 12.0
Industrial Wastewater 7.49 10.0 88.5 ~ 103.7 97.6 ± 9.8
Mg2
Surface water 25.8 10.0 83.6 ~ 104.6 93.8 ± 13.6
Groundwater 5.93 5.00 85.3 ~ 89.9 87.6 ± 3.8
Domestic sewage 0.07 0.20 87.3 ~ 110.6 97.9 ± 16.8
Industrial wastewater 0.93 2.00 92.6 ~ 107.8 101.3 ± 11.6
Note. ND means not detected.
Appendix B
(Informative)
Cationic standard solution chromatogram
Figure B.1 and Figure B.2 show the chromatograms of the cationic standard solutions corresponding to the two reference conditions.
2-Na; 3-NH4
; 4-K; 5-Mg2; 6-Ca2
Figure B.1 Chromatography of six cationic standard solutions (Suppression)
1-Li; 2-Na; 3-NH4
4-Mg2; 5-K; 6-Ca2
Figure B.2 Chromatogram of six cationic standard solutions (non-inhibitory)
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