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Specifications and test procedures for automatic on-line monitoring of mercury in water
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HJ 926-2017
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Basic data | Standard ID | HJ 926-2017 (HJ926-2017) | | Description (Translated English) | Specifications and test procedures for automatic on-line monitoring of mercury in water | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Word Count Estimation | 14,196 | | Date of Issue | 2017-12-28 | | Date of Implementation | 2018-04-01 | | Regulation (derived from) | Ministry of Environmental Protection Bulletin 2017 No. 85 | | Issuing agency(ies) | Ministry of Ecology and Environment |
HJ 926-2017: Specifications and test procedures for automatic on-line monitoring of mercury in water ---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.
People's Republic of China national environmental protection standards
Specifications and test procedures for automatic on-line
monitoring of mercury in water
2017-12-28 Published
2018-04-01 implementation
Directory
Foreword ..ii
1 scope of application .1
2 Normative references .1
3 Terms and definitions .1
4 technical requirements
5 performance indicators and detection methods 5
6 Operating Instructions ..10
Foreword
In order to implement the "Law of the People's Republic of China on Environmental Protection" and the "Law of the People's Republic of China on Prevention and Control of Water Pollution", protect the environment,
Protection of human health, regulate mercury automatic online monitor technical performance, the development of this standard.
This standard specifies the technical requirements, performance indicators and detection methods of mercury automatic online monitor.
This standard is released for the first time.
This standard by the Environmental Protection Department of Environmental Monitoring Division and Science and Technology Standards Division to develop.
This standard was drafted. China Environmental Monitoring Station.
This standard MEP approved on December 28,
This standard since April 1,.2018 come into operation.
This standard is interpreted by the MEP.
Mercury water quality automatic on-line monitor technical requirements and testing methods
1 scope of application
This standard specifies the technical requirements, performance indicators and detection methods of mercury automatic online monitor.
This standard applies to the production of mercury automatic online monitor design, application selection and performance testing.
For applications in different occasions Mercury automatic online water quality monitor (hereinafter referred to as "instrument"), this standard specifies the two types
Instrument range.
The range of type I instruments is 0 ~ 0.002 mg/L, which is mainly used for the monitoring of surface water, groundwater and drinking water.
The measuring range of ІІ type instruments is 0 ~ 0.1 mg/L, which is mainly used for the monitoring of domestic sewage and industrial wastewater.
2 Normative references
This standard references the following documents or the terms. For undated references, the effective version applies to this standard.
GB 4208 enclosure protection (IP code)
GB/T 12519 analytical instruments General technical conditions
HJ 212 Pollutants Online Monitoring (Monitoring) System Data Transfer Standard
HJ 597 Water quality - Determination of total mercury - Cold atomic absorption spectrophotometric method
HJ/T 341 Water quality - Determination of mercury - Cold atomic fluorescence method (Trial)
3 Terms and definitions
The following terms and definitions apply to this standard.
3.1
Indication error
The relative error between the measured value and the true value of the instrument.
3.2
Limit of quantification
The instrument can measure the minimum concentration of the substance under the premise of meeting the indication error requirement.
3.3
Precision precision
Under the specified test conditions, the degree of agreement between the test results of multiple instruments.
3.4
Zero drift zero drift
Under the premise of unplanned manual maintenance and calibration of the instrument, the continuous measurement of the concentration value according to the specified period is the detection
Range of the lower limit of the standard solution, the measured value of the instrument and the initial value of the maximum change relative to the upper limit of the detection range of the relative deviation.
3.5
Range drift rangedrift
Under the premise of unplanned manual maintenance and calibration of the instrument, the continuous measurement of the concentration value according to the specified period is the detection
Range of the upper limit of 80% of the standard solution, the measured value of the instrument and the maximum change between the initial value relative to the detection range
Surrounding the upper limit of the relative deviation.
3.6
Environmental temperature stability
Instrument in different ambient temperature measurement standard solution, the measured value and the reference value of the indication error.
3.7
Ion interference
Instrument to join the interference ion standard solution was measured, the measured value and the true value of the indication error.
3.8
Memory effect
Instrument to complete a standard solution or water samples measured after the next measurement results.
3.9
Spike recovery recovery
Instruments were measured before and after the addition of a certain concentration of the standard solution of the actual water samples, calculated after adding the standard solution measured value
The percentage increase relative to the theoretical amount added.
3.10
Data efficient availability of data
In the minimum maintenance cycle indication error to meet the requirements of the test data as a percentage of all test data.
3.11
Consistent conformity
The degree of parallelism of multiple instruments measured under the same test conditions.
3.12
Minimum maintenance period
In the testing process does not carry out any form of manual maintenance of the instrument (including the replacement of reagents, calibration equipment, maintenance equipment
Etc.) until the instrument can not maintain the normal measurement state or the total running time (h) when the measurement result does not meet the relevant requirements.
3.13
Check with standard solution
Instrument measurement standard solution, to determine the accuracy of measurement results.
3.14
Running log running record
During the operation of the instrument automatically records the test conditions, fault, maintenance and other status information and routine calibration, parameter changes and other maintenance records.
4 technical requirements
4.1 Instrument composition
The basic components of the instrument shown in Figure 1, mainly contains the following units.
Figure 1 The basic components of the instrument
Injecting/measuring unit. Including water sample, standard solution, reagents and other parts of the introduction (aqueous sample channel and standard solution)
And measurement section.
Digestion Unit. A unit that converts mercury and its compounds in a water sample to mercury ions.
Analysis unit. the reaction module and the detection module to complete the automatic analysis of the substance to be tested on the part.
Control unit. including system control hardware and software, control equipment sampling, testing and other components of the process of action, the
Measured value is converted into electrical signal output, complete data processing, transmission part.
4.2 basic requirements
4.2.1 The identification of the instrument shall comply with the requirements of GB/T 12519, the nameplate shall be fixed in an appropriate and obvious place,
Have the following logo.
a) manufacturer's name and address;
b) instrument name, model specifications;
c) factory number;
d) date of manufacture;
e) detection range, lower limit of quantification;
f) Working conditions.
4.2.2 The monitor should be free from stains and damage. All display interface should be Chinese, and the characters are uniform, clear, no hidden corners of the screen,
Dark spots, rainbow, bubbles, flickering and other phenomena, according to the display prompts for full program operation.
4.2.3 chassis shell should be made of corrosion-resistant materials, no cracks on the surface, deformation, pollution, burrs and other phenomena, the surface coating
Uniform, non-corrosive, rusty, peeled and worn.
4.2.4 Product assembly should be strong, no loose parts, buttons, switches, locks and other flexible and reliable components.
4.2.5 The main components should have the corresponding logo or text description.
4.2.6 The analysis flow chart should be identified in the prominent position of the instrument.
4.2.7 The enclosure of the instrument shall meet the IP 52 protection grade requirements of GB 4208.
4.3 Performance Requirements
4.3.1 injection/measurement unit
4.3.1.1 should be anti-corrosion and adsorption of low material composition, not because of reagents or substances to be tested corrosion or adsorption
Measure the result.
4.3.1.2 should ensure the accuracy of the water sample, standard solution, reagents and other injection.
4.3.2 reagent storage unit
Should be able to store all the necessary reagents for the instrument to facilitate replacement, storage temperature 4 ~ 10 ℃, dark.
4.3.3 digestion unit
4.3.3.1 High temperature, high pressure, ultraviolet and other digestion methods should be used to convert all the mercury and its compounds in the water sample into mercury ions.
4.3.3.2 should be anti-corrosion high temperature materials, and easy to clean.
4.3.3.3 should have an automatic heating device and temperature sensor, you can set the digestion time and temperature.
4.3.3.4 There should be a cooling device and safety protection device, can be maintained at constant temperature or constant pressure.
4.3.4 Analysis unit
4.3.4.1 The reaction module should be made of anti-corrosion material, and easy to clean.
4.3.4.2 Detection module output signal should be stable.
4.3.5 Control Unit
4.3.5.1 Should have abnormal information (overrange, lack of reagents, component failure, excessive, etc.) feedback function, should adopt the sound and light alarm.
4.3.5.2 There shall be automatic cleaning of the injection/metering, digestion and analysis units.
4.3.5.3 In case of accidental power failure again after the power should be automatically discharged before the power is measured in the test substances and reagents, automatically clear
Wash each channel and reset to the state where the measurement is restarted. If the heating before digestion in the digestion state, re-energized automatically
Cool down and reset to the state where measurement is restarted.
4.3.5.4 The data processing system shall have such functions as data and operation log acquisition, storage, processing, display and output, etc.
Can store at least 12 months of raw data and running logs, and have the second-level operation and management authority, the average operator can only
Query the corresponding log and instrument setting parameters.
4.3.5.5 The unit of instrument is mg/L or μg/L, and has the function of converting between mg/L and μg/L units.
4.3.5.6 should have automatic standard verification and automatic calibration function, when the automatic standard verification fails, the automatic calibration,
And the results credited to the operation log.
4.3.5.7 should have daily calibration, parameter changes automatically record, save and query functions.
4.3.5.8 should have different test data to add maintenance logo function, such as maintenance. M; fault. D; calibration. C; standard
Kind check. SC.
4.3.5.9 Data transmission Communication protocols shall be provided and the requirements of HJ 212 shall be met.
4.3.5.10 should have a digital communication interface, through the digital communication interface output related data and operation log, and can be accessed
Receive remote control instructions.
4.4 safety requirements
4.4.1 The insulation resistance between the power lead-in cable and the cabinet shall be ≥20 MΩ.
4.4.2 There should be leakage protection devices and overload protection devices to prevent personal electric shock and accidental burning of the instrument.
4.4.3 should have a good grounding port.
4.4.4 High temperature, high pressure, corrosion, toxic and harmful and other dangerous parts should have warning signs.
5 performance indicators and testing methods
5.1 performance indicators
The detection range of type I instrument is 0.00005 ~ 0.002 mg/L; the detection range of ІІ type instrument is 0.002 ~ 0.1 mg/L.
Performance specifications for type I and type ІІ instruments shall comply with the requirements of Table 1.
Table 1 mercury automatic online monitor performance indicators
Performance indicators I type ІІ type
Indication error ± 10% ± 5%
Quantitative lower limit ≤ 0.00005 mg/L ≤ 0.002 mg/L
Precision ≤5% ≤5%
Zero drift ≤2% ≤2%
Drift ≤10% ≤10%
Voltage Stability ± 5% ± 5%
Ambient temperature stability ± 10% ± 10%
Ion interference ± 30% ± 30%
Memory effect ± 10% ± 10%
Spiked recovery 80% ~ 120% 75% ~ 125%
Actual water sample comparison test
When the actual water sample concentration ≤0.0005 mg/L,
The absolute error is not greater than ± 0.0001 mg/L;
The actual water sample concentration > 0.0005 mg/L phase
Error ≤15%;
≤15%
Data efficiency ≥90% ≥90%
Consistency ≤10% ≤10%
Minimum maintenance cycle ≥ 168 h ≥ 168 h
5.2 test conditions
5.2.1 Ambient temperature. 5 ~ 40 ℃
5.2.2 Relative humidity. (65 ± 20)%.
5.2.3 Power supply voltage. AC voltage, (220 ± 22) V.
5.2.4 Power frequency. (50 ± 0.5) Hz.
5.2.5 water sample temperature. 0 ~ 50 ℃.
5.2.6 water pH. pH 6 ~ 9.
5.2.7 Water Suspension. 50 mg/L or less.
5.3 Reagents
5.3.1 Experimental water. Mercury-free distilled water.
5.3.2 Nitric acid (HNO3). ρ = 1.42 g/mL, excellent grade pure.
Mercury standard fixative. potassium dichromate solution ρ (K2CrO7) = 0.5 g/L. Weigh 0.5 g potassium dichromate (K2CrO7, excellent grade pure)
Dissolve in 950 ml of water (5.3.1) and add 50 ml of nitric acid (5.3.2).
5.3.3 Mercury standard stock solution. ρ (Hg) = 1000.0 mg/L.
Weigh 0.1354 g mercuric chloride (HgCl2, superior grade pure) which is fully dried in a silica gel dryer and fixed with mercury standard
After the solution (5.3.3) is dissolved, it is transferred to a 1000 ml volumetric flask, diluted with mercury standard fixative to the mark and mixed.
5.3.4 Calibration fluid. Prepared in accordance with the instructions of the instrument.
5.3.5 Remaining Reagent. Prepare according to the instruction manual of the instrument.
5.4 Experimental Preparation and Calibration
5.4.1 Connect the power, according to the instructions of the instrument, preheat the instrument to normal operation.
5.4.2 In accordance with the instructions of the instrument, calibrate the instrument with calibration fluid.
5.5 test method
5.5.1 indication error
Instruments were the concentration of the upper limit of detection range of 20%, 50% of the standard solution 6 consecutive measurements, calculate each standard
Quasi-solution 6 times the measured value of the average concentration of the known standard solution and the relative error, take two standard solution relative error value
Larger value as the indication error indication.
Standard solution relative error calculation method see formula (1).
5.5.2 Quantitative lower limit
Instrument under the same conditions for the continuous measurement of the concentration of the detection range of the lower limit of the standard solution seven times to calculate seven measurements
Of the standard deviation S, the standard deviation of 10 times the lower limit of quantitative instruments. Calculation method see formula (2) and (3).
5.5.3 Precision
The instrument measures the concentration value of the upper limit of the detection range of 50% of the standard solution, continuous measurement of 6 times, 6 times the measured value of the phase
For the standard deviation, the relative standard deviation was used as the precision judgment value. Calculation method see formula (4).
5.5.4 Zero drift
The concentration of the detection range for the lower limit of the standard solution to 1 h cycle, continuous measurement 24 h, take the first three times the determination
The average of the values is the initial measurement value, and the maximum change width of each measurement value and the initial measurement value is calculated with respect to the detection range
Relative deviation of limits. Calculated by the formula (5) and (6).
5.5.5 Range Drift
The concentration of the detection range for the upper limit of 80% of the standard solution to 1 h cycle, continuous measurement 24 h, take the first 3
The average value of the measured values is the initial measured value, and the maximum change width of each measured value and the initial measured value is calculated with respect to the detection range
Surrounding the upper limit of the relative deviation. Calculated by the formula (7) and (8).
5.5.6 Voltage stability
The concentration of the detection range for the upper limit of 20% of the standard solution, the instrument under the initial voltage of 220 V continuous measurement of 3
Times, the average value of the three measurements for the initial value; adjust the voltage to 242 V, the same standard solution measured 3 times; adjust the voltage to
198 V, measured the same standard solution three times, according to the formula (9) to calculate the relative error caused by voltage changes, take two voltage
Under the relative error of the larger value as a voltage stability of the judge.
5.5.7 Ambient temperature stability
The instrument is placed in a thermostatic chamber, measuring the concentration of the upper limit of the detection range of 20% and 80% of the standard solution, in turn
To 20 ℃, 5 ℃, 20 ℃, 40 ℃, 20 ℃ under 5 constant temperature for 3 h after the measurement results. With 3 20 ℃ conditions
Under the average value of the measured value as a reference value, according to the formula (10) calculated at 5 ℃, 40 ℃ under the two conditions the first measured value and reference
The relative error of the test value, taking the maximum relative error as the temperature of the instrument ambient temperature to determine the value of stability.
5.5.8 Ion interference
Interfering ions specified in Table 2 were added to the standard solution, the mixed solution after the addition of a single interfering ion concentration
Degree should meet the requirements of Table 2, the mercury ion concentration of 50% of the upper limit of the detection range. Instrument were measured three times the mixed solution
Liquid mercury ion concentration, calculated three measurements show the value of the error, whichever is the maximum value of the error as the determination of the instrument ion interference.
Table 2 interference ions and their concentrations
5.5.9 Memory Effect
Instrument 3 consecutive determination of the concentration of the detection range of 20% of the upper limit of the standard solution (test results without assessment), and then
Followed by measurement of the concentration of the upper limit of detection range of 80% and 20% of the standard solution 3 times, respectively, after the calculation of the two standard solutions
The first measured value relative to the true value of the standard solution of the relative error, take the larger the relative error as the instrument memory effect of the judgments.
5.5.10 Spike recovery
Take the actual water samples from the detection of low concentrations of water samples were spiked recovery test. Instrument continuous measurement of water samples 3 times and total
Calculate the average value of the determination, in 1000.0 ml of the same water sample by adding 1.0 ml of mercury standard solution, the instrument continuous measurement of adding standard
After the solution of water samples three times and calculate the average value measured. Calculate the spike recovery R of the actual water sample according to formula (11).
5.5.11 Actual water sample comparison test
Select the three actual water samples, the concentration from low to high coverage of the basic coverage of the instrument, respectively, with the instrument and HJ 597
Or HJ/T 341 method of measurement, each water sample with the number of measurements should not be less than 15 times, using laboratory GB method of measurement
The number of times should not be less than 3 times, in different concentration intervals, respectively, each of the actual value of water samples and laboratory GB method of determination
The average value of the absolute value of the error between the absolute value of the absolute value of the average or absolute value of the instrument as the actual water than the check
Measured error of the judgment value, see calculation formula (12).
5.5.12 minimum maintenance cycle and data efficiency
Instrument 1 h for the cycle of continuous measurement of water samples from the beginning of measurement time, the measurement process does not perform any of the instruments
What form of manual maintenance (including the replacement of reagents, calibration equipment, maintenance equipment, etc.) until the instrument can not maintain the normal measurement
The relative error of the state or three consecutive measurements exceeds ± 10% and the total running time (h) is recorded as the minimum maintenance interval of the instrument.
During this period the efficiency of the data of each instrument should reach more than 90%, data efficiency is the ratio of valid data and all data,
See equation (13).
6 Operating Instructions
The operating instructions of the instrument should include at least the following. instrument principle, instrument structure diagram, test flow chart, on-site safety
Installation conditions and methods, equipment operation methods, parts identification and precautions, toxic and hazardous substances (parts) warning signs, instruments
Calibration reagents and other reagents used in preparation methods and methods of use, troubleshooting, waste disposal methods, routine maintenance instructions.
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