HJ 678-2013 English PDF

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HJ 678-2013: Water quality. Digestion of total metals. Microwave assisted acid digestion method
Status: Valid

Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
HJ 678-2013	269	Add to Cart	3 days	Water quality. Digestion of total metals. Microwave assisted acid digestion method	Valid

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Basic data

Standard ID: HJ 678-2013 (HJ678-2013)
Description (Translated English): Water quality. Digestion of total metals. Microwave assisted acid digestion method
Sector / Industry: Environmental Protection Industry Standard
Word Count Estimation: 10,169
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 total amount of metal in the water pretreatment microwave acid digestion method. This standard applies to surface water, groundwater, sewage and industrial waste water 20 kinds of metal elements in the total acid digestion micr

HJ 678-2013: Water quality. Digestion of total metals. Microwave assisted 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.Microwave assisted acid digestion method National Environmental Protection Standard of the People's Republic Digestion microwave digestion of total water metal Released on.2013-11-21 2014-02-01 implementation release Ministry of Environmental Protection

Content

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

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 ensure human health and standardize microwave digestion methods for total metal in water. This standard specifies the microwave digestion method for the total amount of water metal. 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 microwave digestion of total water metal Warning. The operation of microwave acid digestion must be carried out in a fume hood. Protective gloves and other protective devices should be worn as required. Avoid contact with skin and clothing.

1 Scope of application

This standard specifies the microwave acid digestion pretreatment method for the total amount of metal in water. This standard applies to the microwave acid elimination of the total amount of 20 metal elements in surface water, groundwater, domestic sewage and industrial wastewater. Pretreatment, 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), bismuth (Tl), vanadium (V), zinc (Zn), and the like. 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 is appropriate. Used 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

Microwave acid digestion is a pretreatment technique combined with high pressure digestion and rapid microwave heating. Absorption of water and acid mixture After the microwave energy, the oxidation activity of the acid increases, and the metal element in the sample is released into the solution.

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 newly prepared two. Sub-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. 5.4 Hydrochloric acid. ρ (HCl) = 1.19 g/ml, analytically pure. 5.5 Hydrogen peroxide. ω (H2O2) = 30%. 5.6 Nitric acid solution. 1 1, prepared with nitric acid (5.2). 5.7 Hydrochloric acid solution. 1 1 Prepared with hydrochloric acid (5.4). 5.8 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 (5.7) one by one. Soak for at least 12h. Rinse with distilled water until neutral, dry and seal for use.

6 Instruments and equipment

6.1 Microwave Digestion Apparatus Microwave power can ensure rapid heating, the general power is 600 ~ 1500W; temperature accuracy can reach ± 2.5 ° C; equipped with micro Wave digestion tank. 6.2 Temperature controlled heating equipment. able to maintain the solution temperature at 95 ± 5 °C. 6.3 Centrifugal separator. The speed can reach more than 3000rpm. 6.4 Filtering device. 6.5 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

8.1 Microwave Digester Reference Conditions Heating time. 10 min; digestion temperature. 180 ° C; holding time. 15 min. Note 1. The best measurement conditions of different types of instruments are different, and can be selected according to the instruction manual of the instrument. 8.2 Digestion solution selection Digestion solution 1. 5.0 ml concentrated nitric acid (5.1), suitable for arsenic, calcium, cadmium, cobalt, copper, potassium, manganese, molybdenum, nickel, lead, antimony, Digestion of zinc. Digestion solution 2. 4.0 concentrated nitric acid (5.1) and 1.0 ml concentrated hydrochloric acid (5.3), suitable for silver, aluminum, lanthanum, cerium, chromium, iron, magnesium, Digestion of vanadium elements. 8.3 Operation steps Measure 25 ml of the mixed water sample in a microwave digestion tank, add 1.0 ml of hydrogen peroxide (5.5), and analyze the elements. Select Digestion Solution 1 or Digestion Solution 2, observe the solution, if there is a large amount of air bubbles, put it in a fume hood and let it react smoothly. After the cover is tightened. Place in a microwave digestion apparatus and digest according to the recommended temperature program (8.1). After the program is finished, take out the digestion tank and put it in the fume hood for cooling. After the temperature in the tank is balanced with the room temperature, deflate and open the lid. Remove the in-tank digestion solution, rinse the inner wall of the digestion tank twice with the test water, collect all the solution, and transfer to a 50 ml volumetric flask. Add water to the marking line for testing. Can also be used in the sub-boiling state of the hot plate (maintaining the solution temperature 95 ± 5 ° C), heating and concentration, constant volume Into a 25 ml volumetric flask. Note 2. If there are particles in the sample, use a suction filter (6.4) 0.45 μm acetate filter (5.8) for suction filtration, or at 3000 rpm. Centrifuge for 10 min. 8.4 Blank experiment The experimental water was used instead of the sample to be digested in synchronism with the sample according to the above procedure.

9 Quality Assurance and Quality Control

9.1 The measurement result of the blank experiment is less than the method detection limit. 9.2 Each batch of samples should be tested in parallel with 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. Reason. 10.2 The utensils used in the experiment should be washed with detergent first, then soaked in nitric acid solution (5.6) for 24 h, and then used before use. The tap water and the experimental water are washed and naturally dried. It is strictly forbidden to use chromic acid washing liquid to wash sample bottles and glassware to avoid introducing chromium. Pollution. 10.3 If during the sample digestion process, the pressure is reduced due to excessive pressure in the sample digestion tank, destroying the closed system At this time, the batch sample data is not used.

Appendix A

(informative appendix) Method precision and accuracy The water sample is separated by inductively coupled plasma mass spectrometry and inductive coupling according to the microwave acid digestion method specified in this standard. The measurement was carried out by daughter emission spectroscopy. Six validation laboratories experimented with 20 metal elements in three actual samples Inter-room verification, Table A gives the precision and accuracy indicators such as method repeatability, reproducibility and spike recovery. Schedule A Method Precision and Accuracy Data for Actual Samples Serial number metal name sample Types of Actual sample average value (mg/L) Laboratory interior standard deviation (%) Interlaboratory phase standard deviation (%) Repeatability limit r (mg/L) Reproducibility limit R (mg/L) Spike recovery rate _2% pSp ± 1 Be 1 0.0018* 2.9～5.8 4.2 0.0002 0.0002 89.5±5.1 2 0.0019* 2.2～6.8 2.8 0.0003 0.0001 92.3±3.9 3 0.0019* 1.9～8.8 2.8 0.0003 0.0001 93.9±5.0 2 V 1 0.0019* 2.0～6.0 2.8 0.0002 0.0001 92.8±3.6 2 0.0019* 2.8~6.8 3.0 0.0003 0.0002 92.7±2.9 3 0.0019* 1.4～8.5 2.7 0.0003 0.0001 96.3±5.1 3 Cr 1 74.4 0.1～1.6 1.4 1.91 2.98 93.3±3.0 2 0.088 0.6～5.0 5.3 0.008 0.013 92.5±2.4 3 0.0028 2.8～8.2 8.1 0.0006 0.0006 88.6±5.9 4 Co 1 0.137 0.4～3.1 4.9 0.0073 0.0188 98.9±3.9 2 0.0057 2.8～7.1 6.3 0.0008 0.0010 97.5±2.1 3 0.0019* 2.6～7.7 2.8 0.0003 0.0001 92.9±3.2 5 Ni 1 21.5 0.2～2.8 3.1 0.898 1.85 93.7±2.8 2 0.281 0.2～3.9 5.4 0.015 0.042 91.2±4.8 3 0.030 1.9~7.3 7.6 0.0042 0.0063 92.1±3.7 6 Cu 1 79.5 0.1～1.1 3.5 1.61 7.89 97.5±6.0 2 0.116 0.5～3.1 2.2 0.0062 0.0072 94.8±4.3 3 0.022 3.7～7.7 7.5 0.0034 0.0046 95.0±1.7 7 Zn 1 173 0.3~3.6 6.8 8.32 32.9 96.7±5.0 2 0.497 0.4～2.9 1.6 0.019 0.023 104±9.1 3 0.361 0.4～2.4 3.7 0.014 0.038 98.5±1.9 8 As 1 0.0018* 4.1～6.0 4.6 0.0003 0.0002 88.6±8.9 2 0.0018* 1.9~7.8 3.1 0.0002 0.0002 87.5±7.9 3 0.0018* 2.0～5.9 6.0 0.0002 0.0003 87.1±8.4 Serial number metal name sample Types of Actual sample average value (mg/L) Laboratory interior standard deviation (%) Interlaboratory phase standard deviation (%) Repeatability limit r (mg/L) Reproducibility limit R (mg/L) Spike recovery rate _2% pSp ± 9 Mo 1 0.048 2.6～7.7 8.3 0.0062 0.0112 91.1±3.8 2 0.0019* 3.2～6.4 2.2 0.0002 0.0001 92.7±3.0 3 0.0019* 1.7~7.4 0.0 0.0053 0.0003 95.4±1.9 10 Ag 1 0.569 0.6～5.0 2.3 0.037 0.037 98.0±7.1 2 0.0020* 1.6～5.4 3.2 0.0002 0.0002 99.4±6.4 3 0.0121 3.1～6.8 6.8 0.0016 0.0023 97.3±5.4 11 Cd 1 0.0027 2.9～9.6 9.1 0.0005 0.0007 103±10.9 2 0.0019* 2.3～8.7 0.0 0.0003 0.0000 94.4±3.0 3 0.0018* 1.2～8.7 3.5 0.0003 0.0002 90.6±5.3 12 Ba 1 1.06 0.8～7.2 5.5 0.096 0.164 94.6±5.4 2 0.032 3.5～5.5 6.4 0.0045 0.0058 96.5±3.0 3 0.021 2.5～7.1 7.7 0.0029 0.0046 99.9±3.9 13 Tl 1 0.926 0.2～1.3 1.2 0.022 0.031 101±7.3 2 0.034 3.5～6.9 6.4 0.0054 0.0060 96.3±2.1 3 0.0018* 5.1～7.7 0.0 0.0003 0.0000 98.2±10.8 14 Pb 1 0.460 0.5～1.6 1.7 0.015 0.022 94.4±6.2 2 0.062 1.4～4.7 4.6 0.0057 0.0079 95.2±4.7 3 0.0041 2.8～8.0 5.3 0.0006 0.0006 94.6±3.0 15 Al 1 21.0 0.2 to 3.9 3.3 1.08 1.92 102±6.3 2 0.151 1.8～5.4 5.3 0.015 0.022 102±7.5 3 0.162 0.9～3.5 5.7 0.011 0.026 99.8±6.1 16 Ca 1 14.3 0.4～3.4 2.9 0.703 1.17 94.3±4.5 2 10.3 0.2～3.7 5.2 0.612 1.50 95.8±4.6 3 176 0.4～3.3 2.4 7.04 11.8 100±7.3 17 Fe 1 407 0.1～1.5 0.9 7.38 9.81 93.5±5.9 2 0.379 0.2～3.8 3.5 0.018 0.037 99.8±5.5 3 0.809 0.1～1.0 1.7 0.012 0.040 98.2±3.2 18 K 1 27.9 0.4～2.5 2.2 1.02 1.76 101±7.2 2 7.18 0.3~1.0 0.9 0.119 0.189 94.3±3.2 3 8.97 0.1～1.1 1.1 0.159 0.283 95.9±3.0 19 Mg 1 3.54 0.2～1.4 2.1 0.083 0.211 99.3±3.3 Serial number metal name sample Types of Actual sample average value (mg/L) Laboratory interior standard deviation (%) Interlaboratory phase standard deviation (%) Repeatability limit r (mg/L) Reproducibility limit R (mg/L) Spike recovery rate _2% pSp ± 2 0.957 0.2～2.1 2.1 0.025 0.057 97.6±2.1 3 1.65 0.4～1.9 2.1 0.057 0.099 97.0±3.2 20 Mn 1 1.85 0.2～2.7 4.5 0.075 0.230 98.4±3.2 2 0.023 0.9～8.1 9.2 0.0031 0.0058 98.5±4.0 3 0.162 0.7～3.0 3.4 0.0085 0.0152 96.0±4.1 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 6 parallel measurements after the spike. ......

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