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HJ 1005-2018 English PDF

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HJ 1005-2018: Ambient air - Determination of cations (Na+, NH4+, K+,Mg2+, Ca2+) in precipitation - Ion chromatography
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Basic data

Standard ID HJ 1005-2018 (HJ1005-2018)
Description (Translated English) Ambient air - Determination of cations (Na+, NH4+, K+,Mg2+, Ca2+) in precipitation - Ion chromatography
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z15
Word Count Estimation 14,192
Date of Issue 2018-12-26
Date of Implementation 2019-06-01
Regulation (derived from) Ministry of Ecology and Environment Announcement No. 71 of 2018
Issuing agency(ies) Ministry of Ecology and Environment

HJ 1005-2018: Ambient air - Determination of cations (Na+, NH4+, K+,Mg2+, Ca2+) in precipitation - Ion chromatography


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Ambient air - Determination of cations (Na , NH4 , K , Mg2 , Ca2 ) in precipitation - Ion chromatography National Environmental Protection Standard of the People's Republic Ambient air precipitation cation (Na, NH4) Determination of K, Mg2, Ca2) by ion chromatography Ambient air-Determination of cations (Na , NH4 , K , Mg2 , Ca2 ) In precipitation-Ion chromatography Published on.2018-12-26 2019-06-01 Implementation Ministry of Ecology and Environment released i directory Foreword...ii 1 Scope...1 2 Normative references...1 3 Principles of the method...1 4 Interference and elimination...1 5 Reagents and materials...1 6 Instruments and Equipment...3 7 samples...3 8 Analysis steps...3 9 Calculation and representation of results...4 10 Precision and Accuracy...5 11 Quality Assurance and Quality Control...5 12 Notes...6 Appendix A (informative) Cationic standard solution chromatogram...7 Appendix B (informative) Method Precision and Accuracy...8

Foreword

To protect the "Environmental Protection Law of the People's Republic of China" and the "Air Pollution Control Law of the People's Republic of China" State environment, ensuring human health, standardizing the determination method of cations (Na, NH4, K, Mg2, Ca2) in precipitation Set this standard. This standard specifies ion chromatography for the determination of cations (Na, NH4, K, Mg2, Ca2) in precipitation. Appendix A and Appendix B of this standard are informative annexes. This standard is the first release. This standard is formulated by the Department of Eco-Environmental Monitoring, the Department of Regulations and Standards of the Ministry of Ecology and Environment. This standard was drafted. China Environmental Monitoring Station. This standard is verified by. Liaoning Provincial Environmental Monitoring Experimental Center, Inner Mongolia Autonomous Region Environmental Monitoring Center Station, Taiyuan City Ring Environmental Monitoring Center Station, Nanchang Environmental Monitoring Station, Yangzhou Environmental Monitoring Center Station, Zhanjiang Environmental Protection Monitoring Station and Chongqing Shapingba District Environmental Monitoring Station. This standard is approved by the Ministry of Ecology and Environment on December 26,.2018. This standard has been implemented since June 1,.2019. This standard is explained by the Ministry of Ecology and Environment. 1 ambient air precipitation cation (Na, NH4 , K, Mg2, Ca2) Determination of ion chromatography Warning. The chemical reagents such as nitric acid and methanesulfonic acid used in the experiment have strong corrosiveness and irritancy. The process shall be carried out in a fume hood; the protective equipment shall be worn as required to avoid inhalation of the respiratory tract or contact with skin and clothing.

1 Scope of application

This standard specifies ion chromatography for the determination of cations (Na, NH4, K, Mg2, Ca2) in precipitation. This standard applies to the determination of five cations (Na, NH4, K, Mg2, Ca2) in precipitation. When the injection volume is 25 μl, the detection limits of Na, NH4, K, Mg2, and Ca2 are 0.02 mg/L, respectively. 0.02 mg/L, 0.03 mg/L, 0.02 mg/L and 0.03 mg/L, the lower limit of determination is 0.08 mg/L, 0.08 mg/L, 0.12 mg/L, 0.08 mg/L, and 0.12 mg/L.

2 Normative references

This standard refers to the following documents or their terms. For undated references, the valid version applies to this standard. GB 13580.2 Collection and preservation of atmospheric precipitation samples HJ/T 165 acid deposition monitoring technical specification

3 Principle of the method

The target ions in the precipitation sample are separated from the eluent by the eluent and detected by a conductivity detector. Qualitative, peak height or peak area quantified.

4 interference and elimination

Two kinds of ions with similar retention times can be adjusted by adjusting the flow rate when the concentration difference is large and affects the determination of low concentration ions. Eliminate interference by changing the ratio of eluent.

5 reagents and materials

Unless otherwise stated, the analysis uses a grade of pure reagent that meets national standards. Experimental water is resistivity ≥ 18.2 MΩ·cm (25 ° C), freshly prepared deionized water. 5.1 Nitric acid. ρ (HNO3) = 1.42 g/ml. 5.2 Sodium chloride (NaCl). 2 Dry the constant weight at 105 °C ± 5 °C before use, and store in a desiccator. 5.3 Ammonium chloride (NH4Cl). After drying at 105 ° C ± 5 ° C for constant weight before use, it is stored in a desiccator. 5.4 Potassium chloride (KCl). After drying at 105 ° C ± 5 ° C for constant weight before use, it is stored in a desiccator. 5.5 Calcium chloride (CaCl2). After drying at 105 ° C ± 5 ° C for constant weight before use, it is stored in a desiccator. 5.6 Magnesium chloride (MgCl2). After drying at 105 ° C ± 5 ° C for constant weight before use, it is stored in a desiccator. 5.7 Methanesulfonic acid. w (CH3SO3H) ≥ 98%. 5.8 Nitric acid solution. c (HNO3) = 1 mol/L. Pipette 68 ml of nitric acid (5.1) slowly into water, dilute to 1000 ml with water, and mix. 5.9 Sodium ion standard stock solution. ρ(Na)=1000 mg/L. Accurately weigh 2.5435 g of sodium chloride (5.2) dissolved in a small amount of water, transfer to a 1000 ml volumetric flask, and dilute to volume with water. To the marking line. Transfer to a plastic reagent bottle, sealed at 4 ° C or less, and stored for 6 months. You can also buy a commercially available certificate. standard solution. 5.10 Ammonium ion standard stock solution. ρ(NH4)=1000 mg/L. Accurately weigh 2.9722 g of ammonium chloride (5.3) dissolved in a small amount of water, transfer to a 1000 ml volumetric flask, and dilute to volume with water. To the marking line. Transfer to a plastic reagent bottle, sealed at 4 ° C or less, and stored for 6 months. You can also buy a commercially available certificate. standard solution. 5.11 Potassium ion standard stock solution. ρ (K ) = 1000 mg/L. Accurately weigh 1.9102 g of potassium chloride (5.4) dissolved in a small amount of water, transfer to a 1000 ml volumetric flask, and dilute to volume with water. To the marking line. Transfer to a plastic reagent bottle, sealed at 4 ° C or less, and stored for 6 months. You can also buy a commercially available certificate. standard solution. 5.12 Calcium standard stock solution. ρ(Ca2)=1000 mg/L. Accurately weigh 2.7750 g of calcium chloride (5.5) dissolved in a small amount of water, transfer to a 1000 ml volumetric flask, add 1.00 ml Nitric acid solution (5.8), dilute to the mark with water. Transfer to plastic reagent bottle, cold and light sealed below 4 °C, Save for 6 months. A commercially available certified standard solution can also be purchased. 5.13 Standard stock solution of magnesium ion. ρ(Mg2)=1000 mg/L. Accurately weigh 3.9583 g of magnesium chloride (5.6) dissolved in a small amount of water, transfer to a 1000 ml volumetric flask, add 1.00 ml Nitric acid solution (5.8), dilute to the mark with water. Transfer to plastic reagent bottle, cold and light sealed below 4 °C, Save for 6 months. A commercially available certified standard solution can also be purchased. 5.14 Mixed standard use solution. ρ = 100 mg/L. Pipette 10.00 ml of sodium ion standard stock solution (5.9), ammonium ion standard stock solution (5.10), and potassium ion standard storage Preparation liquid (5.11), calcium ion standard stock solution (5.12) and magnesium ion standard stock solution (5.13) in a 100 ml volumetric flask, Dilute to volume with water. 5.15 eluent 5.15.1 Methanesulfonic acid rinse stock solution. c (CH3SO3H) = 1 mol/L. 3 Pipette 65.0 ml of methanesulfonic acid (5.7) dissolved in an appropriate amount of water, transfer to a 1000 ml volumetric flask, dilute to volume with water line. The solution is stored in a glass reagent bottle and can be stored for 3 months at room temperature. 5.15.2 Methanesulfonic acid leaching solution. c(CH3SO3H)=0.02 mol/L. Pipette 40.0 ml of methanesulfonic acid leaching stock solution (5.15.1) into a.2000 ml volumetric flask and dilute to volume with water. 5.15.3 Nitric acid rinsing solution. c (HNO3) = 4.5 mmol/L. Pipette 9.00 ml of nitric acid solution (5.8) into a.2000 ml volumetric flask and dilute to volume with water. Note. The eluent can also be prepared according to the instrument model and column instructions. 5.16 Water-based microporous membrane. pore size 0.45 μm.

6 Instruments and equipment

6.1 Ion Chromatograph. with conductivity detector. 6.2 Column. 6.2.1 Cation column I. length 250 mm, inner diameter 4 mm, packing is polyacrylic acid, polystyrene/divinylbenzene, etc. A functional group such as a carboxylic acid group or a phosphoric acid group is bonded to the corresponding protective column. Or other equivalent cation column. 6.2.2 Cation column II. length 150 mm, inner diameter 4 mm, filler is silica gel, etc., bonding functional groups such as carboxylic acid groups, Equipped with a corresponding guard column. Or other equivalent cation column. 6.3 Cationic electrolytic regeneration suppressor (optional). 6.4 Vial. Plastic material such as polyethylene. 6.5 Common instruments and equipment used in general laboratories.

7 samples

7.1 Sample Collection Sample collection was carried out in accordance with the relevant provisions of GB 13580.2 and HJ/T 165. The collected sample was filtered through a water microporous membrane (5.16) and transferred to a vial (6.4). 7.2 Sample storage The samples were stored in a refrigerated seal below 4 °C. Among them, NH4 + Complete measurement within 24 h, Na, K, Mg2, Ca2 The assay was completed within 28 days. Note. Solid precipitation samples such as snow water should be filtered and sampled after they are naturally melted. Some samples should not be taken for measurement before they are completely melted.

8 Analysis steps

8.1 Instrument Reference Conditions 8.1.1 Reference condition 1 Cation column I (6.2.1), column temperature. 35 ° C. Methanesulfonic acid rinse solution (5.15.2), flow rate. 1.0 ml/min. Cationic electrolysis regeneration suppressor (6.3), conductivity detector. Injection volume. 25 μl. Determination of target deviation under this reference condition The ion chromatogram obtained from the 4 substandard solution is shown in Figure A.1 in Appendix A. 8.1.2 Reference condition 2 Cation column II (6.2.2), column temperature. 35 ° C. Nitric acid rinse solution (5.15.3), flow rate. 0.9 ml/min. Conductivity detector. Injection volume. 25 μl. The ion chromatogram obtained by measuring the target ion standard solution under this reference condition Figure A.2 in Appendix A. 8.2 Establishment of the standard curve Accurately transfer 0 ml, 0.20 ml, 1.00 ml, 5.00 ml, 10.00 ml, 20.00 ml mixed standard solution (5.14) In a set of 100 ml volumetric flasks, dilute to volume with water and make a reference mass concentration of 0 mg/L. Mixed standard series of 0.20 mg/L, 1.00 mg/L, 5.00 mg/L, 10.0 mg/L, 20.0 mg/L. According to the instrument reference strip Pieces (8.1) are measured sequentially from low to high concentrations. The mass concentration (mg/L) of the target ion is plotted on the abscissa, peak height or The peak area is the ordinate and a standard curve is established. Note 1. The appropriate standard series concentration range can be selected according to the concentration level of the target ion in the sample to be tested. Note 2. When the NH4 is determined by the inhibition conductance method, the standard curve is quadratic; when the non-suppressed conductance method is used to determine NH4, the standard curve is used. One fit. 8.3 Sample determination The measurement of the sample was carried out in accordance with the same conditions and procedures as in the establishment of the standard curve (8.2). If the sample concentration is high At the highest point concentration of the standard curve, the sample can also be diluted and measured, and the dilution factor D is recorded. 8.4 Blank test The sample was replaced with experimental water, and the blank sample was measured in the same conditions and procedures as in the sample measurement (8.3).

9 Calculation and representation of results

9.1 Qualitative analysis Qualitative according to the retention time of the target ions in the sample. 9.2 Calculation of results The mass concentration (mg/L) of the target ions (Na, NH4, K, Mg2, Ca2) in the sample, according to formula (1) Calculation. =ρ Is ×D (1) Where. ρ - the mass concentration of the i-th cation in the sample, mg/L; Is - mass concentration of the ith cation obtained from the standard curve, mg/L; D--Dilution factor of the sample. 59.3 Results are expressed The retention of the number of digits after the decimal point is consistent with the method detection limit, and up to three significant digits are retained. 10 Precision and accuracy 10.1 Precision 7 laboratories have a uniform certificate of concentration of Na, NH4, K, Mg2, and Ca2 from 0.15 mg/L to 2.94 mg/L. The standard sample was tested 6 times. the relative standard deviation in the laboratory was 0.0% to 5.9%; the relative standard between laboratories The deviation was 0.9% to 2.6%; the repeatability limit was 0.02 mg/L to 0.09 mg/L; and the reproducibility limit was 0.02 mg/L to 0.14 mg/L. 7 laboratories added blanks containing Na, NH4, K, Mg2, and Ca2 at concentrations ranging from 0.20 mg/L to 10.2 mg/L The sample was subjected to 6 repeated spikes. the relative standard deviation in the laboratory was 0.0% to 8.5%; the relative standard between laboratories The deviation was 1.3% to 7.8%; the repeatability limit was 0.02 mg/L to 0.31 mg/L; and the reproducibility limit was 0.03 mg/L to 0.95 mg/L. Seven laboratories performed six replicate measurements on two spiked precipitation samples. the relative standard deviation in the laboratory was 0.0% to 5.8%, the relative standard deviation between laboratories is 2.8% to 9.5%, and the repeatability limit is 0.07 mg/L to 0.42 mg/L. Reproducibility limits are from 0.17 mg/L to 1.88 mg/L. For the specific test results of the method precision, see Table B.1 to Table B.3 in Appendix B. 10.2 Accuracy 7 laboratories have a uniform certificate of concentration of Na, NH4, K, Mg2, and Ca2 from 0.15 mg/L to 2.94 mg/L. The standard sample was subjected to 6 replicate measurements. the relative error in the laboratory was -3.8% to 4.6%. Precipitation samples containing Na, NH4, K, Mg2, and Ca2 concentrations from 0.08 mg/L to 10.3 mg/L in 7 laboratories Six repeated spikes were performed and the spiked concentrations of the five target ions ranged from 0.20 mg/L to 10.0 mg/L. spiked recovery 89.0% to 120%. Method Accuracy Refer to Table B.4 to Table B.5 in Appendix B for specific test results. 11 Quality Assurance and Quality Control 11.1 A blank test should be performed before analyzing the sample. At least 1 should be made for every 20 samples or batches (≤20/batch) Blank sample analysis. The target ion content in the blank sample should be below the method detection limit. 11.2 Establish a standard curve using a standard series of at least 6 concentration points (including zero concentration points). The correlation coefficient of the curve should be ≥ 0.995. The standard curve should be determined simultaneously for every 20 samples or batches (≤ 20 cells/batch). 11.3 At least one parallel sample should be measured for every 20 samples or batches (≤20 cells/batch). The relative deviation should be ≤ 15%. 11.4 At least 1 spiked recovery test or certified reference material test should be done for every 20 samples or batches (≤20/batch) set. Among them, the recovery rate of the spiked standard should be controlled between 85% and 120%, and the measured value of the reference material should be in the uncertainty given by it. Inside. 612 Waste Treatment The waste liquid generated in the experiment should be collected centrally, and be identified, classified and managed. 13 Precautions The eluent entering the system should be degassed beforehand to avoid interference and influence of bubbles entering the ion chromatography piping system. Determination.

7 Appendix A

(informative appendix) Cation standard solution chromatogram Figure A.1 and Figure A.2 show the separation of the target ion standard solution by the inhibition conductance method and the non-suppressed conductance method, respectively. Sub-chromogram. Figure A.1 Chromatogram of cation standard solution (inhibition conductance method, ρ=1.00 mg/L) Figure A.2 Chromatogram of cation standard solution (non-suppressed conductance method, ρ=1.00 mg/L)

8 Appendix B

(informative appendix) Method precision and accuracy The precision and accuracy data of the seven laboratory measurements are summarized in Tables B.1 to B.5. Table B.1 Method Precision (certified standard sample) ion name lot number average value (mg/L) Relative standard in laboratory Quasi-bias (%) Relative standard between laboratories Quasi-bias (%) Repeatability limit r (mg/L) Reproducibility limit R (mg/L) Na 202819 1.30 0.2～3.5 0.9 0.06 0.06 NH4.200582 2.94 0.3~1.6 1.4 0.09 0.14 K 202713 1.99 0.2～2.9 1.6 0.08 0.11 Mg2 203013 0.15 0.0～5.9 2.5 0.02 0.02 Ca2 202915 1.56 0.3~3.5 2.6 0.08 0.13 Table B.2 Method precision (blank sample spike) ion name average value (mg/L) Relative standard in the experimental room deviation(%) Relative standard between laboratories Quasi-bias (%) Repeatability limit r (mg/L) Reproducibility limit R (mg/L) Na 0.20 0.0 to 4.4 7.8 0.02 0.05 2.00 0.2~2.2 1.8 0.08 0.13 10.2 0.0 to 1.7 2.6 0.26 0.77 NH4 0.20 0.0 to 6.2 5.0 0.02 0.03 2.05 0.2~2.2 4.8 0.08 0.29 10.2 0.4～1.9 3.1 0.31 0.95 0.21 2.0 to 7.6 3.8 0.02 0.03 2.04 0.2～3.2 2.5 0.12 0.18 10.1 0.0~1.8 1.8 0.28 0.56 Mg2 0.20 0.0 to 8.5 4.8 0.02 0.03 2.01 0.2～4.0 3.2 0.12 0.21 10.0 0.0 to 1.4 1.3 0.21 0.42 Ca2 0.20 0.0 to 5.8 4.7 0.03 0.04 2.08 0.2～4.8 6.7 0.16 0.42 9.91 0.1～2.0 1.5 0.29 0.48 9 Table B.3 Method precision (actual sample spike) ion name Original concentration (mg/L) Standard concentration (mg/L) Standard concentration determination Mean (mg/L) Experimental room relative standard deviation(%) Interlaboratory standard deviation(%) Repeatability limit r(mg/L) Reproducibility limit R(mg/L) Na 0.31～7.01 2.00 2.07 0.4～3.1 4.2 0.08 0.25 10.0 10.3 0.0 to 2.6 3.3 0.42 1.02 NH4 0.37～2.24 2.00 2.06 0.3~2.8 9.5 0.07 0.55 10.0 10.2 0.0 to 3.0 6.5 0.31 1.88 K 0.08～2.44 2.00 2.05 0.6~2.1 2.8 0.08 0.17 10.0 10.4 0.0 to 2.8 2.9 0.40 0.91 Mg2 0.08~1.06 2.00 2.02 0.3~3.6 4.2 0.08 0.25 10.0 10.2 0.4 to 1.7 4.8 0.25 1.38 Ca2 0.69~10.3 2.00 1.95 0.9 to 5.8 4.8 0.15 0.29 10.0 10.2 0.5 to 2.3 5.3 0.38 1.53 Table B.4 Method Accuracy (certified standard sample) ion name lot number average value (mg/L) Relative error in the experimental room RE (%) Final value of relative error between laboratories RE ±2 RES (%) Na 202819 1.30 -0.8~1.5 0.3±1.8 NH4.200582 2.94 -1.0~2.7 0.8±2.8 K 202713 1.99 -1.0～3.0 1.0±3.2 Mg2 203013 0.15 -2.0～4.6 -1.1±5.0 Ca2 202915 1.56 -3.8~3.2 0.3±5.0 Table B.5 Method accuracy (actual sample spike) Target ion name Original concentration (mg/L) spiked concentration (mg/L) Spike recovery (%) Scaling recovery final value ±2 PS (%) Na 0.31～7.01 0.20～10.0 106～120 107±14.0 NH4 0.37～2.24 0.20～2.00 89.0～117 102±21.0 K 0.08～2.44 0.20～2.00 100～115 107±11.4 Mg2 0.08～1.06 0.20～2.00 90.0～110 101±18.8 Ca2 0.69～10.3 2.00～10.0 94.0～111 101±17.8

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