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HJ 832-2017Soil and sediment. Digestion of total metal elements. Microwave assisted acid digestion method (English PDF)

土壤和沉积物金属元素总量的消解微波消解法

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Issued by

Ministry of Ecology and Environment

Level / Type

National · Mandatory

Issue date

July 18, 2017

Implementation date

September 1, 2017

Scope

HJ 832-2017 is the English-translated version of 土壤和沉积物金属元素总量的消解微波消解法.

HJ 832-2017 — This standard specifies the microwave digestion of the total amount of metal elements in soil and sediments.

The method is applicable to arsenic (As), barium (Ba), beryllium (Be), bismuth (Bi), cadmium (Cd), cobalt (Co) Chromium (Cr), copper (Cu), mercury (Hg), manganese (Mn), nickel (Ni), lead (Pb), antimony (Sb), selenium (Se) Vanadium (V) and zinc (Zn) and other 17 kinds of metal elements of the digestion.

If verified, this method also applies to other metal elements the digestion of the total amount of prime.

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Document preview — HJ 832-2017

National Standard of the People's Republic of China

ICS: 13.080
Classification: Z 18

Issued by: Ministry of Ecology and Environment

Preface
1 Scope of application
2 Normative reference documents
3 Principle of the method
4 Reagents and materials
5 Instruments and equipment
6 Samples
7 Sample digestion .2
8 Precision and accuracy
9 Quality assurance and quality control
10 Precautions
Appendix A (informative) method of precision and accuracy

Foreword

For the implementation of the "People's Republic of China Environmental Protection Law" to protect the environment, protect human health, regulate soil and sediment Metal element digestion method, the development of this standard.

This standard specifies the microwave digestion of the total amount of 17 metal elements in soil and sediments.

This standard is the first release.

Appendix A to this standard is an informative appendix.

This standard is organized by the Environmental Monitoring Department of the Ministry of Environmental Protection, the Secretary for Science and Technology Standards.

The main drafting unit of this standard. Sichuan Province Environmental Monitoring Station.

The standard verification unit. Nanjing Environmental Monitoring Center Station, Xinxiang City Environmental Protection Monitoring Station, Ningbo City Environmental Monitoring Heart, Panzhihua City Environmental Monitoring Center Station, Chengdu Environmental Monitoring Center Station and Hunan Province Environmental Monitoring Center Station.

The Environmental Protection Department of this standard approved on July 18, 2017.

This standard has been implemented since September 1, 2017.

This standard is explained by the Ministry of Environmental Protection.

Soil and Sediment Metals Total Digestion Microwave Digestion WARNING. The operation of the microwave acid digestion should be carried out in a fume hood and should be covered with protective equipment to avoid contact with the skin and clothing.

1 Scope of application

This standard specifies the microwave digestion of the total amount of metal elements in soil and sediments.

2 Normative reference documents

The contents of this standard refer to the following documents or their terms. Those who do not specify the date of the reference file, the effective version of the appropriate for this standard.

GB 17378.3 Marine monitoring specification Part III. Sample collection, storage and transportation Technical specification for soil environmental monitoring

3 Principle of the method

Soil or sediment samples and acid mixture of microwave energy absorption, the acid oxidation activity increased at high temperatures, the metal elements in the sample are released into the solution under high pressure conditions.

4 Reagents and materials

Unless otherwise noted, the use of the use of national standards in accordance with the use of excellent pure chemical reagents.

4.1 Experimental water. Newly prepared secondary deionized water or sub-boiling distilled water, resistivity >= 18Mohm · cm (25 °C).

4.2 Nitric acid. rho (HNO3) = 1.42 g/ml.

4.3 Hydrochloric acid. rho (HCl) = 1.19 g/ml.

4.4 hydrofluoric acid. rho (HF) = 1.16 g/ml.

4.5 perchloric acid. rho (HClO4) = 1.67 g/ml.

4.6 nitric acid solution. 1 99, with nitric acid (4.2) preparation.

4.7 nitric acid solution. 1 1, with nitric acid (4.2) preparation.

5 Instruments and equipment

5.1 Microwave digestion device

Using a sealed microwave digestion device, can simultaneously carry out a number of sample pretreatment. General power of 400 ~ 1600 W, induction Temperature control accuracy of ± 2.5 °C, equipped with microwave digestion tank.

Note. The magnetron should be maintained on a regular basis.

5.2 Analysis of the balance. the accuracy of 0.0001 g.

5.3 temperature control heating equipment. temperature control accuracy of ± 5 °C.

5.4 General laboratory equipment and equipment commonly used.

6 Samples

6.1 Collection and storage of samples

With reference to the relevant provisions of HJ/T 166 for soil samples collected and preserved; with reference to the relevant provisions of GB 17378.3 Collection and storage of sediment samples.

6.2 Preparation of samples

According to HJ/T 166 and GB 17378.3, the collected samples were air-dried in the laboratory, broken, 0.15 mm (100 Mesh) nylon sieve, save.

7 Sample digestion

7.1 Digestion method one

7.1.1 Suitable for the digestion of thallium, beryllium, barium, manganese, copper, lead, zinc, cadmium, chromium, nickel, cobalt and vanadium.

7.1.2 Digestion steps

Weigh the powder, sieve the sample 0.25 ~ 0.5 g (accurate to 0.0001 g) placed in the digestion tank, with a small amount of experimental water (4.1) Wetting. In the acid-proof fume hood, 6 ml of nitric acid (4.2), 3 ml of hydrochloric acid (4.3) and 2 ml of hydrofluoric acid (4.4) were added in this order the sample and digestion solution are well mixed. If there is a strong chemical reaction, until the end of the reaction and then tighten the cover. Digest the digestion tank into digestion After the tank holder is placed in the furnace cavity of the microwave digestion device, it is confirmed that the temperature sensor and the pressure sensor are working properly. According to Table 1 the temperature program is microwave digested and cooled after the end of the program. After the temperature in the tank drops to room temperature, remove the digestion in the anti-acid fume hood Cans, slowly depressurization, open the digestion tank cover.

Table 1 Microwave digestion procedure

Temperature rise time Decomposition temperature holding time 7 min at room temperature 120 °C 3 min 5 min 120 160 ° C 3 min 5 min 160 190 ° C for 25 min the solution in the digestion tank was transferred to a polytetrafluoroethylene crucible and the digestion tank and lid were washed with a little experimental water (4.1) and then into the crucible. The crucible is placed on a temperature-controlled heating apparatus (5.3) for conducting acid in a slightly boiling state. Until the liquid into a sticky Thick, take a little cold, with a small amount of nitric acid dropper (4.6) rinse the crucible inner wall, the use of residual temperature dissolved in the crucible wall and then transferred to a 25 ml volumetric flask, and then a small amount of nitric acid (4.6) was pipetted to repeat the above procedure. Wash the liquid and transferred into the volumetric flask, and then use nitric acid (4.6) constant volume to the mark, mix, put it aside for 60 min to take the supernatant to be measured.

Note 1. If the black residue after microwave digestion, indicating that the carbide is not completely digested. Add 2 ml to the crucible on the thermo-heating device (5.3) Nitric acid (4.2), 1 ml hydrofluoric acid (4.4) and 1 ml perchloric acid (4.5) were added and the reaction was carried out for 30 min in a slightly boiling state.

Continued heating to the perchloric acid white smoke exhausted, the liquid into a sticky shape. The above process is repeated until the black carbide disappears.

Note 2. Due to the large amount of organic matter in soil and sediment samples, the amount of nitric acid, hydrochloric acid and hydrofluoric acid used in microwave digestion can be determined according to the actual situation is increased as appropriate.

Note 3. When the measured element content in the sample is low, the sample weighed can be increased to 1 g (accurate to 0.0001 g), microwave digestion of nitric acid, hydrochloric acid and the amount of hydrofluoric acid should also be increased in proportion to the actual situation, or increase the number of digestion.

Note 4. To avoid loss of digestion and safety, the digestion tank must be cooled to room temperature before opening.

7.2 Digestion method two

7.2.1 for arsenic, bismuth, mercury, antimony, selenium element digestion.

7.2.2 Digestion steps

Weigh the powder, sieve the sample 0.25 ~ 0.5 g (accurate to 0.0001 g) placed in the digestion tank, with a small amount of experimental water (4.1) Wetting. In the acid-proof fume hood, add 2 ml nitric acid (4.2), 6 ml hydrochloric acid (4.3), make the sample and digestion solution fully mixed uniform. If there is a strong chemical reaction, until the end of the reaction and then tighten the cover. Will digest the tank into the digestion tank stent into the microwave after the consumer in the chamber of the solution, verify that the temperature sensor and the pressure sensor are working properly. According to Table 2 of the heating procedures for microwave elimination Solution, after the end of the program cooling. To be in the tank after the temperature dropped to room temperature in the anti-acid ventilation cabinet to remove the digestion tank, slowly depressurizing, Open the digestion lid. The solution in the digestion tank was transferred to a 25 ml volumetric flask and washed with a little experimental water (4.1) and the lid and then into the volumetric flask, and then use the experimental water (4.1) constant volume to the marking, mixing, standing 60 min to take the supernatant Liquid to be measured.

Table 2 Microwave digestion procedure

Temperature rise time Decomposition temperature holding time 7 min at room temperature 120 °C 3 min 10 min 120 180 ° C for 15 min

8 Precision and accuracy

8.1 Precision

The six validation laboratories tested five standard samples of ESS-1, ESS-3, GSS-14, GSS-15 and GSD-9, respectively.

The 17 standard elements in the quasi-material were tested for 6 times, and the relative standard deviation in the laboratory was 0.2% ~ 16%.

The relative standard deviations were. 0.6% ~ 12%; repeatability limit. 0.005 mg/kg ~ 39 mg/kg; reproducibility limit. 0 mg/kg ~ 46 mg/kg.

8.2 Accuracy

The six validation laboratories tested five standard samples of ESS-1, ESS-3, GSS-14, GSS-15 and GSD-9, respectively.

The 17 elements in the quasi-material were tested six times with a relative error of -12% to -0.05%.

Details of precision and accuracy are given in Appendix A.

9 Quality assurance and quality control

9.1 The results of the blank experiment should be less than the method detection limit.

9.2 A parallel sample is measured every 20 samples. If the number of samples is less than 20, at least two parallel samples should be made.

9.3 every 20 samples shall be tested for a soil or sediment certified standard sample or certified reference material, the determination should be in the guarantee Value range.

10 Precautions

10.1 The containers used in the experiment should be washed with detergent and then soaked in nitric acid solution (4.7) for 24 h.

Water, experimental water (4.1) washed, naturally dry.

10.2 In the process of sample digestion, due to the sample digestion tank caused by excessive pressure caused by pressure relief, damage to its closed system, the batch sample digestion is invalid.

Appendix A

(Informative)

Method of precision and accuracy Six validation laboratories were tested for six of the five standard samples or 17 of the reference materials in the standard material,

Table A.1 shows the precision and accuracy of the method.

Table A.1 Precision and accuracy of the method

element

sample

Numbering

average value

(Mg/kg)

standard value

(Mg/kg)

Laboratory

Relative standard

deviation(%)

Inter-laboratory

Relative standard

deviation(%)

Repetitive limit r

(Mg/kg)

Reproducibility R

(Mg/kg)

Relative error

Relative error is final value(%) (1) 10.6 10.7 ± 0.8 1.7 to 6.7 2.3 1.1 1.2 -1.4 -1.4 ± 4.5 15.6 15.9 ± 1.3 0.9 to 7.3 2.9 1.9 2.2 -1.7 -1.7 ± 5.6 (3) 8.28 8.4 ± 0.9 1.1 to 7.0 3.6 1.1 1.3 -1.5 -1.5 ± 7.1 (4) 704 716 ± 16 0.8 ~ 3.3 1.2 35 40 -1.7 -1.7 ± 2.4 (3) 424 430 ± 18 0.7 ~ 2.0 2.0 14 27 -1.5 -1.5 ± 3.9 (5) 599 608 ± 13 0.8 ~ 2.5 1.4 24 32 -1.5 -1.5 ± 2.8 (4) 2.68 2.7 ± 0.1 0.8 to 5.2 3.4 0.2 0.3 -0.9 -0.86 ± 6.8 (3) 1.60 1.8 ± 0.3 1.4 to 5.6 5.3 0.2 0.3 -11 to 11 ± 9.4 (5) 2.42 2.44 ± 0.06 0.6 ~ 7.0 1.1 0.2 0 -0.7 -0.68 ± 2.2 (4) 1.15 1.16 ± 0.06 0.5 to 2.7 2.2 0.06 0.09 -1.2 -1.2 ± 4.3 (3) 0.40 0.42 ± 0.04 1.9 to 6.8 5.7 0.06 0.08 -4.8 -4.8 ± 11 (5) 0.332 0.35 ± 0.02 1.6 to 4.7 9.6 0.03 0.09 -5.2 -5.2 ± 18 (1) 0.088 0.083 ± 0.011 1.9 ~ 9.4 6.4 0.01 0.02 5.8 5.8 ± 14 0.049 0.044 ± 0.014 5.1 ~ 12 8.0 0.01 0.02 12 12 ± 18 (3) 0.243 0.26 ± 0.04 1.0 ~ 9.9 11 0.04 0.08 -6.6 -6.6 ± 20 (1) 14.9 14.8 ± 0.7 0.9 to 4.9 2.3 1.2 1.5 0.4 0.45 ± 4.6 (2) 22.1 22.0 ± 1.7 1.1 ~ 4.6 3.2 1.8 2.6 0.6 0.61 ± 6.5 (3) 14.2 14.4 ± 1.2 0.9 to 5.1 3.9 1.3 2.0 -1.3 -1.3 ± 7.7 (1) 55.8 57.2 ± 4.2 1.0 to 4.8 3.3 3.6 6.1 -2.5 -2.5 ± 6.4 (2) 100 98.0 ± 7.1 0.8 to 5.0 6.3 7.0 19 2.3 2.3 ± 13 (3) 83.2 85 ± 7 0.9 to 4.3 3.6 8.1 11 -2.1 -2.1 ± 7.0 (1) 20.6 20.9 ± 0.8 1.0 to 6.1 2.1 2.0 2.2 -1.5 -1.5 ± 4.1 (2) 29.6 29.4 ± 1.6 1.9 to 6.7 4.2 2.7 4.2 0.6 0.62 ± 8.4 (3) 32.0 32 ± 2 0.4 to 3.1 2.1 1.6 2.4 -0.05 -0.05 ± 4.2 (1) 0.017 0.016 ± 0.003 4.7 ~ 14 6.2 0.005 0.005 4.2 4.2 ± 13 (2) 0.114 0.112 ± 0.012 1.5 ~ 7.8 1.1 0.02 0 1.3 1.3 ± 2.2 (3) 0.084 0.083 ± 0.009 1.4 to 11 3.1 0.02 0 0.6 0.60 ± 6.2 Manganese 4 957 963 ± 20 0.2 to 3.2 1.0 39 46 -0.6 -0.59 ± 2.1 element sample Numbering average value (Mg/kg) standard value (Mg/kg) Laboratory Relative standard deviation(%) Inter-laboratory Relative standard deviation(%) Repetitive limit r (Mg/kg) Reproducibility R (Mg/kg) Relative error (%) Relative error is final value(%) (3) 618 620 ± 20 0.4 ~ 3.2 1.4 28 34 -0.3 -0.27 ± 2.7 (5) 683 688 ± 15 0.5 ~ 1.7 0.56 20 21 -0.7 -0.68 ± 1.1 (1) 29.2 29.6 ± 1.8 2.0 to 3.8 2.8 2.4 3.2 -1.2 -1.2 ± 5.6 (2) 34.9 33.7 ± 2.1 0.8 ~ 3.6 5.5 2.3 5.7 3.5 3.5 ± 11 (3) 31.6 32 ± 2 0.6 ~ 4.4 2.8 2.1 3.1 -1.4 -1.4 ± 5.5 (1) 24.0 23.6 ± 1.2 1.2 ~ 15 2.8 4.1 4.2 1.6 1.6 ± 5.8 (2) 33.4 33.3 ± 1.3 1.1 ~ 12 2.5 4.7 4.9 0.2 0.20 ± 5.0 (3) 23.7 23 ± 3 1.7 ~ 13 8.9 3.6 6.7 2.9 2.9 ± 18 (1) 1.01 1.0 1.5 to 16 12 0.3 0.4 1.2 1.2 ± 26 (2) 1.73 1.8 4.1 to 11 9.9 0.4 0.6 -4.1 -4.1 ± 17 (3) 0.792 0.81 ± 0.15 4.6 ~ 12 7.1 0.2 0.2 -2.0 -2.0 ± 17 (1) 0.092 0.093 ± 0.012 1.1 ~ 11 2.5 0.02 0 -0.7 -0.72 ± 5.0 (2) 0.188 0.19 ± 0.03 0.8 ~ 11 4.3 0.04 0.05 -1.3 -1.3 ± 8.4 (3) 0.157 0.16 ± 0.03 1.8 ~ 14 4.0 0.04 0 -1.8 -1.8 ± 7.9 (4) 0.658 0.67 ± 0.04 0.9 to 3.8 1.2 0.05 0.05 -1.7 -1.7 ± 2.3 (3) 0.461 0.49 ± 0.08 1.8 to 5.7 4.9 0.05 0.08 -5.9 -5.9 ± 9.2 (5) 0.622 0.63 ± 0.03 1.2 to 4.2 2.4 0.05 0.06 -1.4 -1.4 ± 4.8 (1) 77.8 77.5 ± 3.1 0.9 to 2.7 2.0 4.1 5.8 0.4 0.43 ± 4.0 (2) 117 116 ± 5 0.9 to 2.4 3.6 6 13 0.9 0.86 ± 7.2 (3) 95.1 97 ± 6 0.5 to 4.1 2.0 5.6 7.3 -2.0 -2.0 ± 3.9 (1) 56.1 55.2 ± 3.4 1.3 ~ 3.6 3.8 3.7 6.8 1.7 1.7 ± 7.7 (2) 90.2 89.3 ± 4.0 0.4 ~ 2.1 2.7 4.0 7.8 1.0 1.0 ± 5.5 (3) 78.7 78 ± 4 0.5 to 2.9 2.8 4.3 7.4 0.9 0.88 ± 5.7

Note 1. (1)ESS-1; (2)ESS-3; (3)GSD-9; (4)GSS-15; (5) GSS-14.

Note 2. The test method used and the elements of the test are as follows. Inductively coupled plasma mass spectrometry. beryllium, barium, cadmium, cobalt, chromium, copper, manganese, nickel, Lead, vanadium, thallium; inductively coupled plasma emission spectrometry. barium, cobalt, chromium, copper, manganese, nickel, lead, vanadium, zinc; graphite furnace atomic absorption Ash, copper, zinc, nickel; atomic fluorescence method. arsenic, bismuth, selenium, antimony, mercury; heat;

Analytical method. Mercury.

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