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The specification for marine monitoring -- Part 5: Sediment analysis
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The specification for marine monitoring. Part 5: Sediment analysis
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Basic data | Standard ID | GB 17378.5-2007 (GB17378.5-2007) | | Description (Translated English) | The specification for marine monitoring -- Part 5: Sediment analysis | | Sector / Industry | National Standard | | Classification of Chinese Standard | A45 | | Classification of International Standard | 07.060 | | Word Count Estimation | 102,149 | | Date of Issue | 2007-10-18 | | Date of Implementation | 2008-05-01 | | Older Standard (superseded by this standard) | GB 17378.5-1998 | | Quoted Standard | GB/T 12763.8; GB 17378.2; GB 17378.3 | | Regulation (derived from) | Announcement of Newly Approved National Standards No. 12 of 2007 (total 112) | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China | | Summary | This Chinese standard applies to analysis of marine sediment monitoring project methods, sample collection, storage, transport, preprocessing, measurement and calculation results and put forward technical requirements. This standard applies to the ocean, coastal, estuary, harbor sediment surveys and monitoring, also apply to coastal waters, harbors, estuaries and dumping of dredged material investigation and monitoring. | GB 17378.5-2007: The specification for marine monitoring -- Part 5: Sediment analysis---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.
The specificatoin for marine monitoring.Part 5. Sediment analysis
ICS 07.060
A45
National Standards of People's Republic of China
Replacing GB 17378.5-1998
Marine monitoring
Part 5. Sediment analysis
Posted 2007-10-18
2008-05-01 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China released
Table of Contents
Introduction Ⅴ
1 Scope 1
2 Normative references 1
3 Terms and definitions
4 1 General Provisions
4 5 Total Mercury
4 5.1 atomic fluorescence spectrometry
5.2 Cold atomic absorption spectrophotometry 6
6 copper 8
6.1 flameless atomic absorption spectrophotometry (continuous determination of copper, lead and cadmium) 8
6.2 Flame atomic absorption spectrophotometry (continuous determination of copper, lead and cadmium) 10
7 lead 12
7.1 flameless atomic absorption spectrophotometry 12
7.2 Flame Atomic Absorption Spectrometry 12
8 Cd 12
8.1 flameless atomic absorption spectrophotometry 12
8.2 Flame Atomic Absorption Spectrometry 12
9 zinc --- flame atomic absorption spectrophotometry 12
10 Cr 13
10.1 flameless atomic absorption spectrophotometry 13
10.2 diphenyl hydrazine spectrophotometry 15
Arsenic 11 17
11.1 Atomic Fluorescence Spectrometry 17
11.2 Arsenomolybdate - crystal violet spectrophotometric 19
11.3 hydride - atomic absorption spectrophotometry 21
11.4 catalytic polarography 23
12 Selenium 25
12.1 fluorospectrophotometry 25
12.2 diaminobenzidine tetrahydrochloride salt spectrophotometric method 27
12.3 catalytic polarography 29
13 31 Oil
13.1 fluorospectrophotometry 31
13.2 UV spectrophotometry 33
13.3 gravimetric method 35
14 666, DDT --- Gas Chromatography 37
15 polychlorinated biphenyls (PCBs) --- GC 41
16 Dieldrin --- GC 43
Sulphides 17 43
17.1 43 Methylene blue spectrophotometric method
17.2 Ion Selective Electrode 47
17.3 Iodimetry 49
18 50 Organic Carbon
18.1 potassium dichromate oxidation - reduction capacity Act 50
18.2 thermal conductivity method 52
--- Moisture content of 19 weight method 54
20 ORP --- potentiometer Act 55
Appendix A (normative) Table 57 records
Annex B (informative) Determination of the project, method and detection limit 80
Annex C (informative) 81 TP --- spectrophotometry
Annex D (informative) TN --- Kjeldahl titration 84
Annex E (informative) organochlorine pesticides --- Capillary Gas Chromatography 87
Annex F (informative) PCBs --- Capillary Gas Chromatography 91
Adjust Annex G (informative) Determination of Florida and the amount of soil adsorption capacity of 95
Figure 1 cold vapor atomic absorption mercury device 7
Figure 2 arsine generation - absorbing means 20
Figure 3 column 39
Figure 4 hydrogen sulfide generation - absorbing means 45
5 semi-micro distillation Nitrogen (Kjeldahl) 46
Table 1 Analysis of samples taken from the sample to check the proportion of 3
Table 2 parallel double sample relative deviation Table 3
Table 3 concentration of each component of organochlorine pesticide standard solution List 38
Table 4 organochlorine pesticides relative retention times 41
Table 5 PCBs relative retention time of each peak 43
Table A. 1 sediment sampling record 57
Table A. 2 single 58 sediment samples to send samples
Table A. 3 sediment samples analysis criteria (work) curve data record (Atomic Fluorescence Spectrometry) 59
Table A. 4 sediment sample analysis records (Atomic Fluorescence Spectrometry) 60
Table A. 5 sediment samples analysis criteria (work) curve data record (spectrophotometry) 61
Table A. 6 sediment sample analysis records (spectrophotometry) 62
Table A. 7 sediment sample analysis criteria (work) curve data record (flameless atomic absorption spectrophotometry) 63
Table A. 8 sediment samples analysis records (flameless atomic absorption spectrophotometry) 64
Table A. 9 sediment samples analysis criteria (work) curve data record (atomic absorption spectrophotometry) 65
Table A. 10 sediment samples standard (work) curve data record (Polarography) 66
Table A. 11 sediment samples analysis records (Polarography) 67
Table A. 12 sediment samples analysis criteria (work) curve data recording (fluorescence spectroscopy) 68
Table A. 13 sediment samples analysis records (fluorescence spectroscopy) 69
Table A. 14 sediment samples analysis records (gravimetric method) 70
Table A. 15 sediment samples 666, DDT, dieldrin analysis records (GC) 71
Table A. 16 sediment samples PCB analysis records (GC) 72
Table A. 17 sediment samples sulfide analytical standards (working) curve data record (sulfide ion selective electrode) 73
Table A. 18 sediment samples analyzed records sulfide (sulfide ion selective electrode) 74
Table A. 19 sediment samples sulfide analysis records (iodometry) 75
Table A. 20 sediment samples of organic carbon analysis records (redox titration) 76
Table A. 21 sediment samples of organic carbon analysis records (thermal conductivity method) 77
Table A. 22 sediment samples oxidation - reduction potential measurement record (potentiometric method) 78
Table A. 23 marine monitoring sediment analysis result report 79
Table B. 1 measurement item, method and detection limit 80
Table C. 1 sediment TP standard curve data record 82
Table C. 2 Analysis of the sediment record 83 TP
Table D. 1 Analysis of sediment samples recorded 86 TN
Table E. 1 marine sediment record of organochlorine pesticides analysis table 90
Table F. 1 of PCBs in marine sediment record sheet 94
Foreword
All technical content in this section is mandatory.
GB 17378 "marine monitoring" is divided into seven parts.
--- Part 1. General;
--- Part 2. Data processing and analysis of quality control;
--- Part 3. Sample collection, storage and transport;
--- Part 4. Seawater analysis;
--- Part 5. Sediment analysis;
--- Part 6. Analysis of the organism;
--- Part 7. Ecological survey of offshore pollution and biological monitoring.
This section GB 17378 Part 5, instead of GB 17378.5-1998 "specification for marine monitoring Part 5. Sediment analysis."
This section compared with GB 17378.5-1998 main changes are as follows.
--- Determination "project, and the method detection limit" to "informative appendix" (1998 edition Chapter 5; this edition of Appendix B);
--- Increasing the overall mercury "Atomic Fluorescence Spectrometry" (see 5.1);
--- Cancel the total mercury "dithizone spectrophotometry" (1998 version 6.2);
--- Increased arsenic "atomic fluorescence assay" (see 11.1);
--- Modified flameless atomic copper, lead and cadmium absorption spectrophotometry, adjusted to "copper, lead and cadmium continuous assay" (1998 version 7.1,8.1,9.1; this version 6.1,7.1,8.1);
--- Modified flame atomic copper, lead and cadmium absorption spectrophotometry, adjusted to "copper, lead and cadmium continuous assay" (1998 version 7.2,8.2,9.2; edition the 6.2,7.2,8.2);
--- Canceled copper "diethyl dithiocarbamate spectrophotometry" (1998 edition 7.3);
--- Canceled the lead "dithizone spectrophotometry" (1998 edition 8.3);
--- Canceled cadmium "dithizone spectrophotometry" (1998 edition 9.3);
--- Canceled zinc "dithizone spectrophotometry" (1998 edition 10.2);
--- Modify the "fluorescence spectrophotometry" (1998 edition 14.1; 13.1 edition) oils;
--- Revise and improve the recording table each test method and as a "normative appendix" (see Appendix A);
Determination and usage --- Florida soil adsorption capacity adjusted to "informative appendix" (1998 edition Appendix A; Excerpts Appendix G);
--- Added "TP assay" (see Appendix C);
--- Added "total nitrogen assay" (see Appendix D);
--- Increased organochlorine pesticides "Capillary Gas Chromatography" (see Appendix E);
--- Added "method of capillary gas chromatography" PCBs (see Appendix F).
Appendix A of this section is normative appendix, Appendix B, Appendix C, Appendix D, Appendix E, Appendix F and Appendix G is an informative annex.
This part by the State Oceanic Administration.
This part of the National Standardization Technical Commission for Oceanography (SAC/TC283) centralized.
This section drafted by. National Marine Environmental Monitoring Center.
The main drafters of this section. mountain - foot plain, Xuheng Zhen, Yu Tao, He Guangkai, Zhaoyun Ying, Fu Yu congregation, Han Dragon, Guan Tao Ming Ong Jian Guo,
Chenwei Yue, Zhang Chunming, Xu Kuncan, Chenbang Long, Gu Guoliang.
This part of the standard replaces the previous editions are.
--- GB 17378.5-1998.
Marine monitoring
Part 5. Sediment analysis
1 Scope
GB 17378 of the provisions of this part of the analysis of marine sediment monitoring programs, sample collection, storage, transport, pretreatment, measurement results and computing technical requirements.
This section applies to ocean, coastal, estuary, harbor sediment surveys and monitoring, but also for investigation and monitoring of coastal waters, bays, estuaries and dumping of dredged material objects.
2 Normative references
The following documents contain provisions which, through reference in this Part of GB 17378, constitute provisions of this part. For dated references,
All subsequent amendments (not including errata content) or revisions do not apply to this section, however,
Encouraged to whether the latest versions of these files according to the parties that this part of agreement. For undated reference documents, the latest versions apply to this section.
GB/T 12763.8 oceanographic survey - Marine Geological Geophysical Survey
GB 17378.2 specification for marine monitoring Part 2. Data processing and quality control analysis
GB 17378.3 specification for marine monitoring Part 3. Sample collection, storage and transportation
3 Terms and Definitions
The following terms and definitions apply to this part of GB 17378.
3.1
Metering vessel volume mark.
3.2
After evaporation of the solvent container, no white smoke when placed at room temperature.
4 General Provisions
4.1 collect sample pretreatment, preparation and preservation
Sample collection, pre-processing, preparation and storage, see GB 17378.3, the specific content and methods of implementation of the following requirements.
4.1.1 collect samples
4.1.1.1 Equipment and tools
Sampling equipment and tools used are as follows.
--- Like disk access or access model. made of hardwood or polyethylene sheet;
--- Sample box, vial (125mL, 500mL grinding mouth jars) and polyethylene bags;
--- Plastic knives, spoons;
--- Beaker. 50mL, 100mL;
--- Other. record forms, labels plastic cards, pencils, markers, steel tape, rubber bands, work diary.
4.1.1.2 Analysis of samples taken
4.1.1.2.1 surface sediment samples taken
Surface sediment samples taken according to the following steps.
--- With a plastic knife or spoon borrow devices from ear cover carefully take the upper part of 0cm ~ 1cm and 1cm ~ 2cm deposits, representing the surface and subsurface. In case of gravel can be mixed within the sample 0cm ~ 3cm layer;
--- Under normal circumstances, each depicting parts of 3 to 4 parts by analysis of samples, depending on the amount of sample analysis project may be. Such as a lack of sample volume, should be taken once;
--- Sediment samples were taken after collection, quickly charged 100mL beaker (about half a cup, and strive to maintain the status quo samples, to avoid air entering) for field measurement with redox potential (also can be directly measured in the dredging vessel);
--- Taking about 5g fresh wet sample, flourished in 50mL beaker for field measurement sulfide (ion selective electrode method). If colorimetric determination of sulfide or by iodometry
Then take 20g ~ 30g fresh wet sample, flourished in 125mL grinding mouth jar plugged after nitrogen filling plug grinding mouth;
--- Take 500g ~ 600g wet sample, has been washed into a polyethylene bag, tie the bag. For the determination of copper, lead, cadmium, zinc, chromium, arsenic and selenium use;
--- Take 500g ~ 600g wet sample, poured into 500mL grinding mouth jar, sealed bottle. For determination of moisture content, size, total mercury, oils, organic carbon, organochlorine pesticides and polychlorinated biphenyls used.
4.1.1.2.2 cylindrical sediment samples taken cylindrical sediment samples taken the following steps.
--- Like columns at 30cm by 5cm intervals within the lower press 10cm intervals (more than 1m at the discretion) cut into small pieces with a plastic knife, carefully scrape the surface of the sample column, three longitudinal cut (ratio of three 1.1.2);
--- Two less are poured into 50mL beaker when sulfide, sulfide as determined by colorimetric assay or iodine (ion selective electrode method,
Then filled in 125mL grinding mouth jar, after sufficient nitrogen, sealed) and polyethylene bags;
--- Another load 125mL grinding mouth jar.
4.1.2 Sample registration, preservation and transportation
Sample registration, preservation and transportation steps are as follows.
--- Vials and polyethylene bags in advance (1 + 3) 2d ~ 3d soaked with a solution of nitric acid, deionized water rinse clean, dry bottle,
Paste sample labels, with a marker of the sea, the station number, level and sampling date written on the label;
--- Sample placed in a polyethylene bag, and fill station number and levels of the tab into the outer bag, tie the bag with a rubber band. Packing in a cool place;
--- All samples should be sampled waters, station number, level, quantity, description of the situation on-site fill in table A. 1;
--- Need to bring the land back to the laboratory samples shall be stored in a cool place, preferably in the refrigerator or freezer and stored at about 4 ℃;
--- Laboratory samples should be sent to the land, when samples, as shown in Table A. 2 asked to fill out to send samples in triplicate. A stay at the end, with the two samples sent to collect the sample units.
Preparation of samples 4.1.3 Analysis
Preparation step of preparing a sample for analysis of samples 4.1.3.1 Determination of heavy metals (copper, lead, cadmium, zinc, chromium, arsenic and selenium) are as follows.
--- Polyethylene bag wet sample to wash and numbered porcelain evaporating dish, placed in 80 ℃ ~ 100 ℃ oven drying process using a glass rod often flip sample and crush the larger pieces, to accelerate the drying;
--- Spreading the dried sample in a clean polyethylene plate, remove gravel and debris particles larger plants and animals. The sample was loaded Ru Manao bowl, each 500mL agate mortar was charged with about 100g dry sample;
--- Agate ball, all through the ground to 160 mesh (96μm) (prior approval of the test to determine the size and number of agate ball milling time and other conditions, is no longer sieved after grinding) in a ball mill.
Agate mortar can also be crushed by hand, with a 160 mesh nylon sieve, cover with plastic lid sieved sample to prevent escape. The sample was milled mix well;
--- Quartering and dividing by dispensing 10g ~ 20g prepared sample into the sample bags (filled in station number of samples, levels, etc.), sent to each laboratory for analysis.
The remaining sample was poured into a grinding mouth glass jar or sealed plastic jar lid, cap tightly, reserved subsample saved;
--- Operator should wear masks and operate under well-ventilated conditions. Crushed sample and sampling and other tools and utensils were first purification treatment, in order to avoid contamination of the sample.
4.1.3.2 Preparation of sample preparation for determination of analytical sample measured oils, organic carbon, organochlorine pesticides and polychlorinated biphenyls in the following steps.
--- The moisture content had been determined, the sample size and total mercury in the post Spreading been cleaned and numbered enamel plate, placed in the indoor cool air, turning from time to time and the sample crushed chunks,
To accelerate the drying, air drying the sample prepared;
--- Spreading the sample which has been dried in a polyethylene plate, remove gravel and debris particles larger plants and animals;
--- In a ball mill to all through 80 mesh (180μm) (in advance by the test conditions, no longer crushed and sieved), can also be manually crushed porcelain mortar,
80 mesh (180μm) sifted metal screen covered with a metal lid. Samples prevent escape. The sample was milled mix well;
--- Quartering and dividing by dispensing 40g ~ 50g prepared sample into the sample bags (filled in station number of samples, levels, etc.), sent to each laboratory for analysis.
4.1.4 Analysis subsample saved
To ensure comparability of the test results of the previous voyage monitoring and quality data for the development of marine environmental protection and scientific accumulation of information,
Good analysis should be properly preserved subsamples to prepare for QA analysis and other purposes.
4.2 regulations and requirements
4.2.1 Analysis of samples drying. The drying temperature and time are not specified, refer to (105 ± 1) ℃, drying 2h.
4.2.2 Standard Solution, a flask and used pipettes should advance capacity correction or verification.
4.2.3 Data processing executed according to GB 17378.2 requirements.
4.2.4 In addition to the text within the pH measurement method other than stated, or widely available precision measuring pH test paper.
4.2.5 Determination of sulfide deposits not like double check.
4.3 Analysis of the results of quality checks
QA analysis results as follows.
--- The results in Table 1 QA checks randomly selected samples were bagged and another kind of number series, basic kind of analysis and inspection of sample cross-testers were measured;
Table 1 Analysis of samples taken from the check-like proportions
Analysis of the number of samples < 10 10-30> 30
Check sample extraction ratio /% 504 030
--- Check the kind of test items and basically the same kind;
--- When the number of the sample more basic kind of like checking arrangements should be tested in the same batch;
--- Test results are listed in Table 2 Dual-like relative deviation allowable limit quality control analysis, when a two-sample test results measured item super slip greater than 30%
This batch of samples of the basic observation items should all be re-measured. If the above still-tolerance conditions, analysis and testing should be carefully checked analyze the reasons (such as preparation of standard solution,
Environmental quality, used equipment has no unusual circumstances, etc.), and then measured the sample batch (basic sample and check samples) of;
--- When a test sample test results exceed double entry error rate of less than 30%, the sample should be re-called ultra-poor samples were measured until the measurement result qualified so far. Times data, according to the results of parallel double sample mean calculated;
--- Analysis of each batch of samples (20 or so) into 2 ~ 3 marine sediment composition analysis standard substance (respectively bagging and other series like numbers), to test whether the system error.
Table 2 parallel double sample relative deviation table
The results where the magnitude 10-410-510-6 10-710-810-9
Relative deviation allowable limit /% 4815203040
4.4 Description
4.4.1 various chemical density (ρ), is the number of grams per milliliter at 20 ℃.
4.4.2 In addition to the items listed ship-site determination of equipment used, the laboratory determination of land within the project, list only the main equipment and special equipment and utensils.
4.4.3 desiccant when not indicate a specific name, refer to color gel.
4.4.4 concentration of the standard elements are formulated refers to the concentration of the element.
4.4.5 does not specify solvent solution is an aqueous solution.
4.4.6 In addition to electrochemical analysis, calibration curve can also be used linear regression equation, mass or concentration of the analyte, then the formula to calculate the content of the analyte in the sample.
When a middle point of the calibration curve exception is large, the calculation using the linear regression equation content can cause large errors,
It should give up this point, for use as the law required results. As outliers appears across the calibration curve, the range of the calibration curve is correspondingly smaller, it should be redrawn when the calibration curve.
The particle size was measured by deposits 4.4.7 GB/T 12763.8 execution.
5 Total Mercury
5.1 Atomic Fluorescence Spectrometry
5.1.1 Scope and Application
This method is applicable to the determination of freshwater and seawater stream sediments of total mercury.
This method is a method of arbitration.
5.1.2 The principle of the method
Samples of nitric acid - hydrochloric acid system, placed in boiling water bath for digestion, the total amount of mercury as ions into solution. With potassium borohydride as reducing agent, the solution ionic mercury into mercury vapor.
Argon as a carrier gas of atoms of mercury vapor into the atomic fluorescence spectrometer of atomic reactor to special mercury hollow cathode lamp as the excitation source, the determination of mercury atomic fluorescence intensity.
5.1.3 Reagents and preparation
5.1.3.1 nitric acid (HNO3). ρ = 1.42g/mL, pure class distinctions.
5.1.3.2 hydrochloric acid (HCl). ρ = 1.19g/mL, pure class distinctions.
5.1.3.3 potassium borohydride (KBH4).
5.1.3.4 potassium hydroxide (KOH). pure class distinctions.
5.1.3.5 oxalic acid (H2C2O4 · 2H2O).
5.1.3.6 Potassium permanganate (KMnO4).
5.1.3.7 potassium hydroxide solution (0.05g/L). Weigh 1g of potassium hydroxide (see 5.1.3.4) was dissolved in 200mL of deionized water,
Boron was added 0.5g of potassium hydride (see 5.1.3.3) Pipette 20mL dissolved in 1000mL volumetric flask, dilute to the mark with deionized water. Preparation before use.
5.1.3.8 potassium permanganate solution (1%). Weigh 5g of potassium permanganate (see 5.1.3.6) was dissolved in 500mL of deionized water, placed in a brown reagent bottle to save.
5.1.3.9 oxalic acid solution (1%). Weigh 10g of oxalic acid (see 5.1.3.5) was dissolved in 1000mL of deionized water, placed in a brown reagent bottle to save.
5.1.3.10 nitric acid solution (1 + 19). 1 part of nitric acid (see 5.1.3.1) and 19 parts of water are mixed.
5.1.3.11 mercury standard stock solution (1.00g/L). Weigh accurately 0.1353g mercuric chloride (HgCl2, reference reagents or pure class distinctions,
Pre-positioned more than 24h) in sulfuric acid dryer in 50mL beaker, dissolved with a small amount of nitric acid solution (see 5.1.3.10), the total amount transferred to 100mL volumetric flask,
In nitric acid solution (see 5.1.3.10) set the volume to the mark, and mix.
5.1.3.12 mercury standard intermediate solution A (10.0mg/L). Pipette 1.00mL mercury stock standard solution (see 5.1.3.11) into 100mL
Flask, add nitric acid solution (see 5.1.3.10) set the volume to the mark, and mix.
5.1.3.13 mercury standard intermediate solution B (0.100mg/L). Pipette 1.00mL mercury intermediate standard solution A (see 5.1.3.12) placed
100mL flask, add nitric acid solution (see 5.1.3.10) set the volume to the mark, and mix.
5.1.3.14 mercury standard solution (10.0μg/L). Pipette 10.00mL mercury intermediate standard solution B (see 5.1.3.13) into 100mL
Flask, add nitric acid solution (see 5.1.3.10) set the volume to the mark, and mix. Preparation used.
5.1.4 instruments and equipment
Instruments and equipment are as follows.
--- Atomic fluorescence spectrometer;
--- Volumetric flask. capacity of 50mL, 100mL, 1000mL;
--- Pipette. Volume 1mL, 2mL, 5mL, 10mL;
--- Beaker. the capacity of 50mL, 100mL;
--- Water bath;
--- Argon;
--- Commonly used laboratory instruments and equipment.
5.1.5 Analysis of step
5.1.5.1 standard curve
5.1.5.1.1 in seven 100mL flask were added 50mL of deionized water was added 10mL of nitric acid (see 5.1.3.1) and
10mL of concentrated hydrochloric acid (see 5.1.3.2), then were added mercury standard solution (see 5.1.3.14) 0mL, 0.25mL, 0.50mL,
1.00mL, 2.00mL, 4.00mL, 8.00mL, water volume to the mark, and mix.
5.1.5.1.2 mercury were taken above the standard series solution of 2mL, measurement standard blank fluorescence intensity readings (I0) and standard sample fluorescence intensity readings (Ii).
5.1.5.1.3 The data recorded in Table A. 3, the fluorescence intensity (Ii-I0) for the vertical axis, the amount of mercury (ng) as the abscissa, the standard curve
(Given in linear regression equation) and calculate the linear regression coefficients.
5.1.5.2 sample determination
5.1.5.2.1 accurately weighed 0.1g ~ 0.5g dry sediment samples or 1g ~ 5g wet sediment sample (accurate to 0.0001g), placed
50mL stoppered colorimetric tube, add 2mL nitric acid (see 5.1.3.1), 6mL hydrochloric acid (see 5.1.3.2). With approximately 10mL of deio...
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