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HJ 442.4-2020 English PDF

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HJ 442.4-2020: (Technical specifications for environmental monitoring in coastal waters - Part 4: Sediment monitoring in coastal waters)
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GB 8702   HJ 630   HJ 607   HJ 442.1   HJ 442.2   HJ 442.10   

Basic data

Standard ID HJ 442.4-2020 (HJ442.4-2020)
Description (Translated English) (Technical specifications for environmental monitoring in coastal waters - Part 4: Sediment monitoring in coastal waters)
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z06
Classification of International Standard 13.020
Word Count Estimation 15,127
Date of Issue 2020-12-16
Date of Implementation 2021-03-01
Older Standard (superseded by this standard) HJ 442-2008
Regulation (derived from) Ministry of Ecology and Environment Announcement No. 66 [2020]
Issuing agency(ies) Ministry of Ecology and Environment

HJ 442.4-2020: (Technical specifications for environmental monitoring in coastal waters - Part 4: Sediment monitoring in coastal waters)


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(Technical specifications for environmental monitoring in coastal waters Part 4 Sediment monitoring in coastal waters) National Environmental Protection Standards of the People's Republic of China Replace HJ 442-2008 Technical specifications for environmental monitoring in coastal waters Part Four. Monitoring of Sediment in Coastal Seas Technical specification for offshore environmental monitoring Part 4 offshore sediment monitoring 2020-12-16 release 2021-03-01 implementation Issued by the Ministry of Ecology and Environment i table of contents Foreword...Ⅱ 1 Scope of application...1 2 Normative references...1 3 General requirements for sediment quality monitoring in coastal waters...1 4 Collection, storage and transportation of sediment samples...2 5 Preparation of sediment samples...4 6 Sediment sample analysis...4 7 Quality control of sediment monitoring...5 Appendix A (informative appendix) Analysis method of coastal sediment quality monitoring project...7 Appendix B (informative appendix) Sediment total nitrogen-potassium persulfate oxidation method...9 Appendix C (informative appendix) Sediment total phosphorus-potassium persulfate oxidation method...11

Foreword

To implement the Environmental Protection Law of the People’s Republic of China, the Marine Environmental Protection Law of the People’s Republic of China, and the "Regulations on the Administration of the Prevention and Control of Land-Source Pollutants Pollution and Damage to the Marine Environment" of the People’s Republic of China "Regulations on the Management of Pollution Damage to the Marine Environment" and "Administrative Measures for Environmental Functional Zones in Coastal Sea Areas" to regulate the quality of the ecological environment in the coastal sea Monitoring, protecting the ecological environment, and ensuring the scientific, accurate, systematic, comparable and representative It is indicative of this standard. This standard was first published in.2008.The original standard drafting unit was China Environmental Monitoring Station and Zhoushan Marine Biotechnology Environmental Monitoring Station. This is the first revision. The revised standard consists of the following ten parts. Part One General Provisions Part Two. Data Processing and Information Management Part III Water Quality Monitoring of Inshore Waters Part Four. Monitoring of Sediment in Coastal Seas Part V Monitoring of Biological Quality in Coastal Waters Part VI Biological Monitoring in Inshore Waters Part VII Monitoring of rivers entering the sea Part 8.Monitoring of Direct Discharge of Sea Pollution Sources and Impact on the Water Environment of Inshore Waters Part IX Emergency and Special Monitoring in Coastal Waters Part 10 Evaluation and Report This standard is the fourth part of the revised standard. The revision mainly focuses on the collection and The methods and procedures of preservation, transportation, laboratory analysis, and quality control are mainly revised in the following aspects. --Adjusted required test items and selective test items; --Added relevant standard analysis methods and requirements that can be selected; --Improved related requirements related to quality management, and increased self-control requirements for analysts; - Two analytical methods have been added as informative appendices. Appendix A, Appendix B and Appendix C of this standard are informative appendices. From the date of implementation of this standard, the "Environmental Monitoring Specifications for Coastal Sea Areas" (HJ 442-2008) shall be abolished. This standard was formulated by the Department of Ecological Environment Monitoring and the Department of Regulations and Standards of the Ministry of Ecology and Environment. Drafting organizations of this standard. China National Environmental Monitoring Station, Zhejiang Zhoushan Marine Ecological Environment Monitoring Station, Tianjin Ecological Environment Environmental Monitoring Center, Dalian Ecological Environment Monitoring Center of Liaoning Province. This standard was approved by the Ministry of Ecology and Environment on December 16, 2020. This standard will be implemented on March 1, 2021. This standard is interpreted by the Ministry of Ecology and Environment.

1 Technical specifications for environmental monitoring in coastal waters

Part Four. Monitoring of Sediment in Coastal Seas

1 Scope of application

This standard specifies the basic methods for the collection, preservation, transportation, laboratory analysis and quality control of sediment samples in coastal seas. Laws and procedures. This standard is applicable to the collection, pretreatment, laboratory analysis, quality of sediment samples in offshore, estuaries and salty and brackish waters. Control work.

2 Normative references

The content of this standard refers to the terms in the following documents. For undated references, the effective version is applicable to this standard. GB 17378.3 Marine Monitoring Specification Part 3.Sample Collection, Storage and Transportation GB 18668 Marine sediment quality HJ 168 Technical Guidelines for the Preparation and Revision of Environmental Monitoring and Analysis Methods HJ 442.1 The general rules of the first part of the technical specifications for environmental monitoring in coastal waters HJ 442.2 Technical Specification for Environmental Monitoring in Coastal Seas Part 2 Data Processing and Information Management HJ 442.10 Technical Specifications for Environmental Monitoring in Coastal Seas Part Ten Evaluation and Report HJ 730 Technical Specification for Layout of Environmental Monitoring Points in Coastal Waters

3 General requirements for quality monitoring of sediments in coastal waters

The implementation plan for routine monitoring of sediments in coastal seas is formulated and implemented in accordance with the relevant requirements of HJ 442.1, and the layout of monitoring points is in accordance with HJ 730 related requirements are implemented, data processing and data reporting shall be implemented in accordance with HJ 442.2 requirements, evaluation and reporting shall be implemented in accordance with HJ 442.10 Seek execution. The frequency of routine monitoring of sediments in important estuaries, bays and key areas as determined by the state is once a year, and in other areas According to the monitoring conditions and evaluation requirements, it can be performed once a year or once every two years. The sampling time is generally arranged in July to August. Combine water quality monitoring. The compulsory items for routine monitoring of sediments in coastal seas are the items with the limits specified in GB 18668 and total phosphorus and total nitrogen; Test items include waste and color (olfactory, structure), coliform, fecal coliform, pathogen, redox potential, sedimentation Type of deposits, etc. Sediment monitoring items, time, frequency, etc. in other monitoring are determined according to the monitoring purpose. 24 Collection, preservation and transportation of sediment samples 4.1 Sample collection 4.1.1 Sampler and auxiliary equipment a) Sediment sampler Generally, it is required to be made of steel with high strength and good wear resistance. The grease should be removed and cleaned before use. root According to different needs, digging (grab) dredgers, cone (drilling) dredgers, tubular dredgers and box mining can be used. Mud. Among them, the excavation type (grab type) mud dredger is suitable for collecting large area surface samples; the cone type (drill type) mud mining The trap is suitable for collecting less sediment samples; the tubular dredger is suitable for collecting cylindrical samples; the box-type dredger is suitable for Collection of large area and certain depth sediment samples. b) Auxiliary equipment Generally include winches (electric or hand-cranked winches), sample trays (made of wood or plastic), plastic knives, spoons, beakers, Record forms, plastic label cards, pencils, markers, steel tapes, sample boxes, etc. 4.1.2 Sample container selection and handling The containers used to store sediment samples are mainly wide-mouth borosilicate glass bottles, polyethylene bags or polystyrene bags (or containers). a) Polyethylene and polystyrene containers are suitable for storage of trace metal samples; b) The brown wide-mouth glass bottle as a container can be used for wet sample measurement items and the storage of sulfide and other samples. Polyethylene bags should not be used for product storage; sediment samples used for organic analysis should be placed in brown glass bottles. The cover should be lined with clean aluminum foil or polytetrafluoroethylene film; c) The strength of the polyethylene bag is limited. Two bags can be used for double-layer reinforcement. A new bag should be used without any printing Logo and handwriting; d) The sample container must be soaked in (1 2) nitric acid for 2 to 3 d before use, washed with deionized water, and (1 2) hydrochloric acid Soak for 2 d, rinse with deionized water, and dry. 4.1.3 Surface sample collection operation Surface sediment samples are generally collected by excavator. Specific operation. connect the mud picker to the end of the wire rope, check Check whether it is reliable, measure the water depth at the sampling point; start the winch slowly, lift the open mud picker, and put it into the water slowly with your hand. After stabilization, put it at a constant speed to 3 m～5 m from the bottom, then put it into the bottom at full speed, then lift the mud dredger slowly, and lift it quickly after leaving the bottom; Lower the mud picker to the sampling tray, open the ear cover of the mud picker, tilt the mud picker to make the upper water flow out slowly, and then make a qualitative description And sub-packaging. Analytical samples of surface sediments are generally taken from the top 0 cm～2 cm sediments. Refer to Table 1 for the sampling amount. Like a one-time pick The sample volume is insufficient and should be sampled again. 4.1.4 Collection of columnar samples The vertical section sediment samples were collected with a gravity sampler. Specific operation. a) After the ship arrives at the sampling point, first collect surface sediment samples to understand the type of sediment. If it is sandy, it is not suitable to collect pillars Shape b) Connect the sampling pipe to the winch and check if it is firm; c) Start the winch slowly, hold the lower end of the sampling tube with your hand and carefully send it outboard of the ship, and slowly put it into the water with a hook; d) After the sampling pipe is stopped in the water, lower it to a distance of 5 m～10 m from the bottom at a constant speed, depending on gravity and sediment type Depending on the type, then plunge into the sediment at full speed; e) Raise the sampling pipe slowly, and then quickly raise it to the surface after leaving the seabed, and then slow down and raise it after exiting the water surface. Stop immediately after the end is higher than the ship’s rail, hook the pipe body with an iron hook to turn it into the ship’s rail and place it flat on the deck; f) Carefully pour out the accumulated water on the upper part of the tube, measure the sampling depth, and then slowly squeeze out the columnar sample and place it in the sample receiving box in order To describe and process; g) Clean the sampling tube and prepare it for use; if the length of the columnar sample is not enough or the gravity sampling tube is inserted into the sediment obliquely, Resample the situation. After the sediment column samples pass through the segments, they are used to monitor the sedimentation rate and pollution status in different years. Generally based on monitoring sea The sediment settling rate of the field and the needs of the pollutant survey of the age, determine the interval of the sample column, use a plastic knife to divide and Section samples are divided into several parts longitudinally for monitoring and analysis of corresponding items. 4.2 On-site description of samples Before the sample is divided, make a description of the color, smell, thickness, and type of the sediment in time, and record it in detail record. 4.3 Marking and recording of samples The sample bottle is numbered in advance, and the label is attached after loading the sample, and the station number is written on the container with a marker to prevent the label from falling off and messing up the sample The product; the plastic bag needs to be marked (note that the zinc oxide tape will cause zinc contamination to the sample and should not be used), and use the written Put the label in the bag and seal it; carefully make a detailed record of the sampling. 4.4 Storage and transportation of samples The collected samples are divided and stored according to the storage conditions in the table below. The sample container should be tightly closed to avoid any Contamination or evaporation. Take care to prevent the container from breaking during transportation. The sample size and storage conditions of sediment samples are shown in Table 1. 45 Sediment sample preparation 5.1 Preparation of heavy metal samples a) Transfer the wet sample in the polyethylene bag to a cleaned and numbered porcelain evaporating dish, and place it in an oven at 80℃～100℃, During the drying process, a glass rod should be used to turn the sample frequently and crush large samples, or use exhaust air to dry, or Directly place the sample in a freeze dryer and freeze-dry it; b) Spread the dried sample on a clean polyethylene plate, crush the sample with a glass rod or polyethylene rod to remove gravel Stones and larger-grained remains of plants and animals. Put the sample into the agate bowl, put the agate ball, and smash on the ball mill To all pass 160 meshes. It can also be crushed by hand in an agate mortar, and sieved with a 160 mesh nylon sieve to prevent samples Product escape c) Mix the processed sample thoroughly, divide it into quarters to divide 10 g～20 g, and put it into the numbered sample bag (corresponding It is equipped with sampling station number, time and other related information records) and sent to the laboratory for analysis and determination. The remaining samples Sheng Put in a 250 ml polyethylene bottle, close the stopper tightly, and save as a copy; d) During preparation, the tools and utensils used should be prepared in advance to avoid contamination of the sample. Under protective conditions; e) The sample preparation for mercury analysis in sediments is carried out in accordance with 5.3 a). 5.2 Preparation of samples for determination of organic matter a) Spread the sample in a cleaned and numbered enamel tray, place it in a cool and ventilated place indoors, flip the sample from time to time And crush the large pieces to speed up the drying to make air-dried samples, or directly put the samples in a freeze dryer to freeze-dry; b) Spread the dry sample on a polyethylene plate, crush the sample with a polyethylene rod, and remove gravel and large particles. Plant remains c) Crush on a ball mill or manually pulverize with a porcelain mortar until all passes through an 80 mesh metal sieve. Prevent samples from escaping; d) Mix the processed samples thoroughly, divide them into 40 g～60 g, and put them into the sample bag (the bag is filled with the sample Station number, level and other related information), sent to each laboratory for analysis and determination. The remaining samples are filled into 250 ml ground mouth For glass bottles, close the cork tightly and save as a copy. 5.3 Other a) Before analyzing the mercury in the sediment, you can choose to freeze the wet sample in a freeze dryer, or at 40℃～60℃ Dry it down and treat it according to the preparation method of heavy metal samples; it can also be directly measured with wet samples and determine the moisture content of the samples. Rate calculated as dry weight; b) Before analyzing the total phosphorus and total nitrogen of the sample, prepare it according to the preparation method of the organic matter sample. Drying is optional Dry at 40℃～60℃ or put the wet sample in a freeze dryer for freeze-drying treatment; c) The drying method of the analysis samples of other projects, according to the degree of temperature influence of the project and the requirements of the method, choose freezing Freeze-drying, natural air-drying and heating drying methods in the dryer, or directly determine and determine the moisture content of the sample by using a wet sample The rate is treated as dry weight calculation. 56 Sediment sample analysis 6.1 Method selection The monitoring analysis method is selected in accordance with the requirements of 6.5.1 of HJ 442.1.Common on-site testing and laboratory analysis methods see attached Record A. 6.2 Method verification and validation In accordance with the relevant requirements of HJ 442.1, when the method and conditions of the first use change, carry out the method verification and conformity After meeting relevant requirements, it can be used for sample determination.

7 Quality control of sediment monitoring

7.1 Basic requirements The basic requirements of organization, personnel, equipment, etc. shall be implemented in accordance with relevant regulations of HJ 442.1. 7.2 Quality control of sample collection Sediment sample collection quality control, according to GB 17378.3 method to collect on-site double samples and prepare them as close to on-site samples Characteristic solid synthetic quality control samples should account for more than 10% of the total samples. When the total number of samples is less than or equal to 10 At that time, only one sample can be collected and produced. 7.3 Laboratory quality control The laboratory's analytical personnel self-control and internal laboratory control shall be carried out according to the following requirements. a) Carry out method verification and validation as required; b) The quality control of sediment analysis generally adopts methods such as laboratory parallel sample analysis and standard sample analysis for quality Control; if the method requires the recovery rate of standard addition, it can be controlled by adding standard recovery sample; c) The self-control of the analyst generally adopts the clear code sample control, and the other control in the laboratory can use the password and the clear code; d) The other control laboratory adopts the random sampling of inspection samples from the samples according to the proportion in Table 2, and the sample numbers are separately assigned to the original samples. Equivalent testing and other laboratory control; e) The allowable value of relative deviation of parallel double samples of sediments (including random samples), and the analysis method shall be as required by the analysis method Implementation is required. If there is no requirement, follow Table 3; the qualification rate of each batch of parallel double samples is above 90%, and the analysis results are Effective; 30% of the samples are randomly selected for re-examination when the pass rate is 70% to 90%, and the re-examination results are generally qualified with the original results When the rate is over 90%, the result is valid; when the pass rate is between 50% and 70%, 50% of the samples should be rechecked, and the total When the grid rate is more than 90%, the result is valid; when the qualified rate is less than 50%, all re-analysis should be performed until the result is consistent. Up to 6 cells; when reporting data, generally report the measured value of each parallel double sample or the mean value of the parallel double sample, and the parallel double sample The calculation of the mean value shall be carried out in accordance with the relevant regulations of HJ 442.2; f) Each batch of samples controlled by the laboratory should insert 2 to 3 marine sediment reference materials/standard samples or quality control samples for analysis Analysis, used to check whether there are systematic errors. When the number of samples is small, it should not be less than 1; generally according to the adopted standard Quasi-method requirements and standard scope of reference materials/standard samples or quality control samples; g) The analyst refers to the analysis method adopted by HJ 168 to determine the effective number of data The last digit is consistent with the last digit of the detection limit effective digits, and the effective data digits are consistent with the requirements; h) The data audit controlled by other laboratories shall be conducted in accordance with the relevant requirements of HJ 442.2.

9 Appendix B

(Informative appendix) Sediment total nitrogen-potassium persulfate oxidation method B.1 Scope of application This method is suitable for the determination of total nitrogen in sediments of estuaries and coastal waters. B.2 Principle of the method Marine sediment samples are oxidized with potassium persulfate under alkaline and 110℃～120℃ conditions, organic nitrogen compounds, Nitrate nitrogen and ammonium nitrogen are converted into nitrate nitrogen. After the digestion is completed, take the upper clear digestion solution and pass it through the copper-plated cadmium reduction column. Nitrate in the buffer solution is reduced to nitrite. Under acidic conditions, nitrite is combined with sulfonamides and N-(1-naphthyl)- Ethylenediamine hydrochloride undergoes a diazoazo reaction to form a nitrogen-containing dye with a maximum absorption at 540 nm. The concentration of this substance The degree is proportional to the original total nitrogen concentration in the sediment. B.3 Reagents and standards Unless otherwise specified, all reagents used are of analytical grade, and the experimental water is double distilled water or equivalent pure water. B.3.1 Sodium hydroxide solution. c (NaOH) = 1.0 mol/L. Weigh 20.0 g of sodium hydroxide (NaOH) into a 1000 ml beaker, add 500 ml of water, boil for 5 minutes, and cool Then make up to 500 ml with water and store in a polyethylene bottle. The sodium hydroxide used must pass the total nitrogen reagent blank value test before it can be used. B.3.2 Potassium persulfate solution. ρ(K2S2O8)= 50.0 g/L. Weigh 5.0 g potassium persulfate (K2S2O8), dissolve it in 50 ml sodium hydroxide solution (B.3.1), and dilute with water to 100 ml, stored in a polyethylene bottle. This solution is stable for 7 days when stored at room temperature and protected from light; it is stable for 30 days when stored at 4℃～6℃ in the dark. The potassium persulfate used must be tested for the blank value of the reagent. If the blank value of the total nitrogen does not meet the requirements, it can be repeated multiple times Crystal method purification. Note. Purification method of potassium persulfate. add about 800 ml of water to a 1000 ml jar, heat in a 30℃ water bath, and gradually add potassium persulfate. Until it can not be dissolved. Place the completely dissolved saturated solution at room temperature and let it cool naturally (use a jar with a lid, avoid introducing Other pollution), then put it in the refrigerator at 4℃ to recrystallize (it needs to be placed overnight or more than 12 hours). The recrystallization is generally twice. Pour out the supernatant after washing, Then put it in an oven at 30℃ to dry. B.3.3 Hydrochloric acid solution. c(HCl)= 1.5 mol/L. Measure 12.5 ml of concentrated hydrochloric acid (HCl, ρ = 1.19 g/ml) into 87.5 ml of water, and mix well. B.3.4 Nitrate stock solution. ρ=100 mg/L, calculated as N. In a 1000 ml long neck volumetric flask, add 800 ml pure water to dissolve 0.7217 g potassium nitrate (dry at 105°C for 1 h), Dilute to the mark with pure water. Store the stock solution in a polyethylene bottle in a refrigerator at 4°C. The solution is stable for 6 months. B.3.5 Nitrate use liquid. ρ=100 mg/L, calculated as N. Dilute 10 ml of nitrate stock solution (B.3.4) to 100 ml with pure water and prepare on the same day. B.4 Instruments and equipment B.4.1 Medical portable steam sterilizer or household pressure cooker. The pressure can reach 1.1 kPa～1.4 kPa, and the temperature can reach 120℃～124℃. B.4.2 Digestion bottle. Teflon bottle or polypropylene bottle with screw cap (60 ml-100 ml). B.4.3 Related equipment for nitrate determination (cadmium column reduction method or continuous flow analysis method). B.5 Analysis steps B.5.1 Preparation of reagents and standards used. B.5.2 Sample digestion. Weigh an appropriate amount (0.200 g～0.500 g) of the sediment sample (after drying and grinding) in a digestion bottle, Add 20.0 ...

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