HJ 677-2013 English PDF

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HJ 677-2013: Water quality. Digestion of total metals. Nitric acid digestion method
Status: Valid

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HJ 677-2013	239	Add to Cart	3 days	Water quality. Digestion of total metals. Nitric acid digestion method	Valid

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Basic data

Standard ID: HJ 677-2013 (HJ677-2013)
Description (Translated English): Water quality. Digestion of total metals. Nitric acid digestion method
Sector / Industry: Environmental Protection Industry Standard
Word Count Estimation: 9,938
Quoted Standard: HJ/T 91; HJ/T 164; HJ 493
Regulation (derived from): Ministry of Environmental Protection Notice No. 70 of 2013
Issuing agency(ies): Ministry of Ecology and Environment
Summary: This standard specifies the amount of nitrate in the water digestion metal pretreatment. This standard applies to surface water, groundwater nitrate, sewage and industrial waste water 20 kinds of metal elements in the total digestion pretreatment, includi

HJ 677-2013: Water quality. Digestion of total metals. Nitric acid digestion method

---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.Digestion of total metals.Nitric acid digestion method National Environmental Protection Standard of the People's Republic Digestion of the total amount of water metal Released on.2013-11-21 2014-02-01 implementation Ministry of Environmental Protection released

Content

Foreword. II 1 Scope 1 2 Normative references 1 3 Terms and Definitions..1 4 Principle of the method 1 5 reagents and materials..1 6 instruments and equipment..2 7 samples..2 8 digestion step 2 9 Quality Assurance and Quality Control. 2 10 Notes. 2 Appendix A (informative) The precision and accuracy of the method..3

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 This standard is formulated to protect human health and standardize the pretreatment method of total metal in water. This standard specifies the nitric acid digestion pretreatment method for the total amount of metal in water. This standard is the first release. Appendix A of this standard is an informative annex. This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection. This standard is mainly drafted by. Ningbo Environmental Monitoring Center. The standard verification unit. Shanghai Environmental Monitoring Center, Hangzhou Environmental Monitoring Center Station, Shaoxing Environmental Monitoring Center Station, Taizhou Environmental Monitoring Center Station, Ningbo Entry-Exit Inspection and Quarantine Bureau and Ningbo Environmental Monitoring Center. This standard was approved by the Ministry of Environmental Protection on November 21,.2013. This standard has been implemented since February 1,.2014. This standard is explained by the Ministry of Environmental Protection. Digestion of the total amount of water metal Warning. The digestion operation must be carried out in a fume hood. Wear protective gloves and other protective equipment as required to avoid contact with the skin. Skin and clothes.

1 Scope of application

This standard specifies the nitric acid digestion pretreatment method for the total amount of metal in water. This standard applies to the total amount of 20 metal elements in surface water, groundwater, domestic sewage and industrial wastewater. Treatment, including silver (Ag), aluminum (Al), arsenic (As), beryllium (Be), barium (Ba), calcium (Ca), cadmium (Cd), cobalt (Co), Chromium (Cr), copper (Cu), iron (Fe), potassium (K), magnesium (Mg), manganese (Mn), molybdenum (Mo), nickel (Ni), lead (Pb), T (Tl), vanadium (V), zinc (Zn). Other metal elements are also valid for this method after verification.

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 Preservation and Management of Water Quality Samples

3 Terms and definitions

The following terms and definitions apply to this standard. Total metal Refers to the metal content determined after digestion of the unfiltered water sample.

4 Principle of the method

At 95 ± 5 ° C, the metal element in the water sample is converted to a single high valence state by oxidation of nitric acid and hydrogen peroxide or It is converted into an inorganic compound that is easy to separate, the organic matter in the sample is destroyed, and the sample is uniformly clear.

5 reagents and materials

Unless otherwise stated, the analysis uses the superior purification reagents that meet the national standards, and the experimental water is the second preparation of the new preparation. Deionized water or sub-boiling distilled water, resistivity ≥ 18MΩ · cm (25 ° C). 5.1 Nitric acid. ρ(HNO3) = 1.42 g/ml. 5.2 Nitric acid. ρ (HNO3) = 1.42 g/ml, analytically pure. 5.3 Hydrochloric acid. ρ(HCl) = 1.19 g/ml, analytically pure. 5.4 Hydrogen peroxide. ω (H2O2) = 30%. 5.5 Nitric acid solution. 1 1, prepared with concentrated nitric acid (5.2). 5.6 Hydrochloric acid solution. 1 1 Prepared with concentrated hydrochloric acid (5.3). 5.7 0.45 μm cellulose acetate filter. Using the edge of the stainless steel tweezers coated with polyethylene film, immersed vertically into the hydrochloric acid solution (5.6) one by one, at least Soak for 12h. Rinse with distilled water until neutral, dry and seal for use.

6 Instruments and equipment

6.1 Temperature-controlled heating equipment. various heating devices capable of controlling the solution temperature in the range of 95±5°C 6.2 Filtering device. 6.3 Centrifugal separator. The speed can reach more than 3000rpm. 6.4 Common instruments and equipment used in general laboratories.

7 samples

7.1 Sample collection and preservation Water samples were collected and stored according to HJ/T 91, HJ/T 164, and HJ 493.

8 digestion steps

Measure 50 ml of the mixed water sample in a 150ml beaker or conical flask, add 5 ml of concentrated nitric acid (5.1), and place it in temperature control. On the heating equipment (6.1), cover the surface dish or small funnel, keep the temperature of the solution at 95±5 °C, and heat it for 30 minutes without boiling. Remove the watch glass and evaporate until the solution is about 5 ml to stop heating. After cooling, add 5 ml concentrated nitric acid (5.1) and cover. The upper watch glass is heated to reflux. If brown smoke is formed, repeat this step (add 5 ml of concentrated nitric acid each time), straight Until there is no more brown smoke, the solution is evaporated to about 5 ml. After the solution is cooled, slowly add 3 ml of hydrogen peroxide (5.4), continue to cover the watch glass, and keep the solution temperature. 95±5 °C, heating until no more bubbles are generated. After the solution is cooled, continue to add hydrogen peroxide (5.4), each time 1 ml, Until only the fine bubbles or the general appearance does not change, remove the watch glass and continue heating until the solution volume evaporates to about 5ml. After the solution is cooled, rinse the inner wall with an appropriate amount of water for at least 3 times, transfer to a 50 ml volumetric flask and dilute to volume. Note. If there are particles in the sample, use a suction filter (6.2) 0.45μm acetate filter (5.7) for suction filtration, or at.2000-3000 rpm. Centrifuge for 10 min at the speed of rotation. Blank experiment. replace the sample with experimental water according to the above steps and digest the sample synchronously.

9 Quality Assurance and Quality Control

9.1 The results of the blank test cannot be greater than the detection limit. 9.2 Each batch of samples should be tested in parallel from 10% to 20%. 9.3 Each batch of samples should be tested for spiked recovery of 10% to 20%. 10 Precautions 10.1 When the blank test result is higher than the method detection limit, the reagent should be screened or the reagent should be purified. 10.2 The utensils used in the experiment should be washed with detergent first, then soaked in nitric acid solution (5.5) for 24 h, and then used before use. Wash water, experiment with water, and dry naturally. It is strictly forbidden to use chromic acid washing liquid to wash sample bottles and glassware to avoid introducing chromium contamination.

Appendix A

(informative appendix) Method precision and accuracy The water sample is sent by inductively coupled plasma mass spectrometry and inductively coupled plasma according to the pretreatment method specified in this standard. The spectroscopy method was used for the measurement. Six laboratories conducted interlaboratory verification of 20 metal elements in three actual samples. Table A.1 gives the precision and accuracy indicators for method repeatability, reproducibility, and spike recovery. Schedule A.1 Method accuracy and accuracy data for actual samples Serial number metal name sample Types of Actual sample average value (mg/L) Experimental room relative standard deviation(%) Interlaboratory standard deviation(%) Repeatability limit r (mg/L) Reproducibility limit R (mg/L) Spike recovery rate _2% pSp ± Be 1 0.0018 * 3.2 to 9.0 8.0 0.0003 0.0001 88.3 ±5.80 2 0.0018 * 2.5～9.4 6.0 0.0003 0.0002 90.8 ±5.02 3 0.0019* 4.1～6.8 5.6 0.0003 0.0002 91.4 ±5.44 2 V 1 0.0018* 2.5～9.4 8.2 0.0003 0.0002 92.3 ±6.68 2 0.0019* 4.2～8.9 12.6 0.0004 0.0002 91.4 ±4.88 3 0.0019* 3.8～7.3 5.6 0.0003 0.0002 94.3±8.58 3 Cr 1 71.1 0.1～1.6 2.0 1.91 4.30 93.9±3.24 2 0.091 1.4～3.2 6.2 0.0067 0.0153 92.5±7.66 3 0.0028 0.6～7.8 7.1 0.0004 0.0004 89.4 ±6.42 4 Co 1 0.141 0.4～3.0 3.9 0.0076 0.0161 98.4±5.86 2 0.0057 0.3～5.2 5.9 0.0005 0.0007 96.5 ±8.38 3 0.0018* 4.2～7.1 2.9 0.0003 0.0002 90.7 ±5.48 5 Ni 1 22.4 0.2～2.0 5.7 0.829 3.86 94.9±7.44 2 0.273 0.2～4.0 4.5 0.131 0.0337 91.9 ±7.64 3 0.028 1.9～3.6 4.9 0.0023 0.0046 90.6 ±6.84 6 Cu 1 79.4 0.1 to 0.7 4.7 1.15 10.8 97.3 ± 7.18 2 0.110 0.4～3.1 5.7 0.0052 0.0177 94.8±4.32 3 0.022 3.5～7.4 7.5 0.0031 0.0023 92.2 ±4.56 7 Zn 1 154 0.3 to 2.0 6.3 5.29 24.7 96.3 ±6.28 2 0.481 0.1～1.1 1.0 0.0091 0.0136 104 ±5.54 3 0.362 0.2～1.6 5.0 0.0100 0.0455 98.9 ±6.92 8 As 1 0.0018* 3.5～9.0 6.9 0.0003 0.0002 86.9±4.96 2 0.0018* 2.2～7.7 9.4 0.0003 0.0002 87.1±5.82 3 0.0017* 5.0～7.8 3.2 0.0003 0.0001 85.8±4.52 9 Mo 1 0.050 2.1～3.3 8.1 0.0037 0.0114 91.9 ±7.46 2 0.0019* 4.0～7.8 6.2 0.0003 0.0002 93.8±8.22 3 0.0019* 3.8～7.1 4.0 0.0003 0.0001 94.9 ±3.90 10 Ag 1 0.552 0.1～2.6 2.0 0.0196 0.0292 99.1±7.58 2 0.0020* 3.2～7.6 4.9 0.0003 0.0002 99.4±6.80 3 0.0121 2.3～6.9 7.1 0.0014 0.0023 89.8 ±5.14 11 Cd 1 0.0032 3.5～5.3 5.2 0.0004 0.0006 99.5 ±6.16 Schedule A.1 Method accuracy and accuracy data for actual samples Serial number metal name sample Types of Actual sample average value (mg/L) Experimental room relative standard deviation(%) Interlaboratory standard deviation(%) Repeatability limit r (mg/L) Reproducibility limit R (mg/L) Spike recovery rate _2% pSp ± 2 0.0019* 4.3～8.1 6.7 0.0003 0.0001 94.0 ±2.32 3 0.0018* 2.0～6.0 5.5 0.0002 0.0002 89.5 ±6.02 12 Ba 1 1.20 0.0 to 3.0 9.7 0.0602 0.322 92.4 ±6.62 2 0.021 1.2～7.0 6.0 0.0018 0.0015 92.2±7.12 3 0.020 2.0 to 5.5 5.1 0.0025 0.0015 99.4 ±6.58 13 Tl 1 0.924 0.2～1.3 2.2 0.0175 0.0631 98.8±7.12 2 0.034 3.4~6.9 5.1 0.0041 0.0074 92.2 ±5.70 3 0.0020* 3.3～7.3 5.3 0.0003 0.0001 99.3±4.60 14 Pb 1 0.473 0.2～2.0 3.0 0.0203 0.0401 94.4 ±6.20 2 0.056 1.9～4.0 5.6 0.0043 0.0058 90.9 ±4.82 3 0.0041 3.0~4.8 5.6 0.0004 0.0008 94.5±5.02 15 Al 1 20.4 0.0 to 2.4 3.8 0.676 2.30 102±5.76 2 0.144 0.4～5.4 7.4 0.0119 0.0295 101±8.12 3 0.171 0.5～3.0 6.3 0.0101 0.0264 99.2 ±5.80 16 Ca 1 15.3 0.3~2.4 9.7 0.695 4.43 94.3 ±4.46 2 9.81 0.0～1.8 4.0 0.233 1.02 93.9 ±9.22 3 172 0.0 to 0.7 1.3 2.53 4.57 98.2 ± 6.92 17 Fe 1 15.0 0.1 to 0.6 2.2 4.32 24.5 93.5 ± 5.90 2 0.383 0.6～1.9 3.8 0.0124 0.0393 99.1 ±6.54 3 0.941 0.5～0.8 6.7 0.0165 0.188 94.8 ±4.26 18 K 1 26.4 0.2～1.2 2.1 0.563 1.44 98.9±7.36 2 7.08 0.1～1.2 1.0 0.143 0.209 91.7 ±6.90 3 8.79 0.1～1.1 3.2 0.152 0.773 94.9 ±2.12 19 Mg 1 3.34 0.2～2.4 3.3 0.121 0.309 98.3 ±9.42 2 0.915 0.1～0.4 0.6 0.0084 0.0133 97.6 ±2.08 3 1.5 0.4～2.4 3.8 0.0508 0.136 95.3 ±2.88 20 Mn 1 1.84 0.2～2.0 3.7 0.0637 0.185 95.5±3.80 2 0.023 1.5～7.5 15.0 0.0029 0.0081 99.2±9.12 3 0.156 1.0～3.0 1.1 0.0091 0.0096 92.0 ±6.36 Note 1.1 electroplating wastewater; 2 papermaking wastewater; 3 surface water Note 2. * means that the actual water sample is not detected, and the precision data is the result of parallel measurement after 6 additions. ......

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