HJ 999-2018Solid waste - Determination of fluoride - Alkali fusion - ion selective electrode method (English PDF)
固体废物 氟的测定 碱熔-离子选择电极法
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Issued by
Ministry of Ecology and Environment
Level / Type
National · Mandatory
Issue date
December 26, 2018
Implementation date
June 1, 2019
Scope
HJ 999-2018 is the English-translated version of 固体废物 氟的测定 碱熔-离子选择电极法.
HJ 999-2018 — Warning. The hydrochloric acid used in the experiment is highly volatile and corrosive, and the sample preparation process should be carried out in a fume hood; Wear protective equipment as required to avoid direct contact with skin and clothing.
1 Scope of application this standard specifies the alkali fusion-ion selective electrode method for the determination of fluorine in solid waste. This standard applies to the determination of fluorine in solid waste.
When the sample is solid or can be dried in a semi-solid state, the sample volume is 0.25 g, and when 10.0 ml of the digestion solution is taken, the side is measured.
The detection limit of the method for determining fluorine is 0.03 g/kg, and the lower limit of determination is 0.12 g/kg. When the sample is liquid or semi-solid without drying State, the sampling amount is 10 g, and when the 10.0 ml digestion solution is removed, the detection limit of the method for measuring fluorine is 0.5 mg/kg. The lower limit of determination is 2.0 mg/kg.
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Document preview — HJ 999-2018
National Standard of the People's Republic of China
- Classification
- Z 13
Issued by: Ministry of Ecology and Environment
Contents
- Foreword
- 1 Determination of fluorine in solid wastes Alkali fusion-ion selective electrode method
- 2 Normative references
- 3 Terms and definitions
- 4 Principle of the method
- 5 Interference and elimination
- 26 Reagents and materials
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 this standard is formulated to protect the ecological environment, ensure human health, and regulate the determination of fluorine in solid waste.
This standard specifies the alkali fusion-ion selective electrode method for the determination of fluorine in solid waste.
This standard is the first release.
This standard is formulated by the Department of Eco-Environmental Monitoring, the Department of Regulations and Standards of the Ministry of Ecology and Environment.
This standard was drafted. Tianjin Ecological Environment Monitoring Center.
The verification unit of this standard. Yunnan Environmental Monitoring Center Station, Hunan Environmental Monitoring Center Station, Shandong Province Environmental Monitoring Xinzhan, Nanjing Environmental Monitoring Center Station, Tianjin Huanke Testing Technology Co., Ltd. and Tianjin Municipal Domestic Waste Inspection heart.
This standard is approved by the Ministry of Ecology and Environment on December 26, 2018.
This standard has been implemented since June 1, 2019.
This standard is explained by the Ministry of Ecology and Environment.
1 Determination of fluorine in solid wastes Alkali fusion-ion selective electrode method
Warning. The hydrochloric acid used in the experiment is highly volatile and corrosive, and the sample preparation process should be carried out in a fume hood;
Wear protective equipment as required to avoid direct contact with skin and clothing.
1 Scope of application this standard specifies the alkali fusion-ion selective electrode method for the determination of fluorine in solid waste.
This standard applies to the determination of fluorine in solid waste.
When the sample is solid or can be dried in a semi-solid state, the sample volume is 0.25 g, and when 10.0 ml of the digestion solution is taken, the side is measured.
The detection limit of the method for determining fluorine is 0.03 g/kg, and the lower limit of determination is 0.12 g/kg. When the sample is liquid or semi-solid without drying State, the sampling amount is 10 g, and when the 10.0 ml digestion solution is removed, the detection limit of the method for measuring fluorine is 0.5 mg/kg.
The lower limit of determination is 2.0 mg/kg.
2 Normative references
This standard refers to the following documents or their terms. For undated references, the valid version applies to this standard.
HJ/T 20 Industrial solid waste sampling and preparation technical specifications HJ/T 298 Hazardous Waste Identification Technical Specification
3 Terms and definitions
The following terms and definitions apply to this standard.
Fluoride
Refers to the fluoride (measured as F) measured after the sample has been extracted by sodium hydroxide under the conditions specified in this standard.
4 Principle of the method
The fluorine in the sample is extracted by high-temperature melting of sodium hydroxide, and is separated by fluorine at a certain pH range and total ionic strength.
The sub-selective electrode method determines that the logarithm of the fluoride ion concentration in the solution is linear with the electrode potential within a certain concentration range.
5 Interference and elimination
When the concentration of Al3 in the sample is higher than 60 mg/L and the concentration of Fe3 is higher than 150 mg/L, the determination of fluorine is negative.
Disturbance can be eliminated by dilution.
26 Reagents and materials
Analytically pure reagents in accordance with national standards were used for analysis, unless otherwise stated. The experimental water was deionized water.
6.1 Hydrochloric acid. rho(HCl) = 1.19 g/ml.
6.2 Sodium hydroxide (NaOH).
6.3 Sodium citrate (Na3C6H5O7·2H2O).
6.4 Citric acid (C6H8O7).
6.5 Bromocresol purple (C21H16Br2O5S).
6.6 Sodium fluoride (NaF).
Bake in an oven at 105 ° C ~ 110 ° C for 2 h, placed in a desiccator, cooled to room temperature, and set aside.
6.7 Sodium hydroxide solution. c (NaOH) = 5 mol/L.
Weigh 100 g of sodium hydroxide (6.2), dissolve in water, dilute to 500 ml, and mix.
6.8 Sodium hydroxide solution. c (NaOH) = 0.2 mol/L.
Weigh 0.8 g of sodium hydroxide (6.2), dissolve in water, dilute to 100 ml, and mix.
6.9 Hydrochloric acid solution. 1 1.
Measure 100 ml of hydrochloric acid (6.1) and dilute to.200 ml with water.
6.10 Total ionic strength adjustment buffer solution (TISAB).
Weigh 294 g of sodium citrate (6.3) and 26 g of citric acid (6.4), add about 900 ml of water to dissolve, and dissolve with hydrochloric acid.
Adjust the pH to about 5.5 with liquid (6.9) or sodium hydroxide solution (6.7), dilute to 1000 ml, and mix. Stored in polyethylene the bottle is stored in a refrigerator at 4 ° C, taken out at the time of use, and used after being placed at room temperature.
6.11 Fluorine standard stock solution. rho (F) = 1000 mg/L.
Accurately weigh 0.22 g (accurate to 0.1 mg) of sodium fluoride (6.6), dissolve in water, and transfer to a 100 ml volumetric flask.
Dilute to the mark with water, mix and store in a polyethylene bottle. Commercially available certified reference materials are also available.
6.12 Fluorine standard use solution. rho (F) = 50.0 mg/L.
Accurately remove 5.00 ml of fluorine standard stock solution (6.11), place in a 100 ml polyethylene volumetric flask, and dilute to the standard with water.
Line, mix.
6.13 bromocresol purple indicator. rho (C21H16Br2O5S) = 0.4 g/L.
Weigh 0.10 g of bromocresol purple (6.5), dissolve in 10 ml of sodium hydroxide solution (6.8), and dilute to 250 ml with water.
6.14 Qualitative filter paper.
7 Instruments and equipment
7.1 Ion meter or acidity meter. resolution 0.1 mV.
7.2 Fluoride ion selective electrode and reference electrode (or fluoride ion composite electrode).
7.3 Magnetic stirrer and polyethylene magnetic stirrer.
7.4 Muffle furnace. room temperature ~ 800 ° C.
7.5 Electric heating plate. It has temperature control function and can set the temperature not lower than.200 °C.
7.6 Ultrasonic cleaner. frequency (40 kHz~60 kHz), temperature can be displayed.
7.7 Nickel. 50 ml or 100 ml with lid.
37.8 Sampling bottle. 250 ml polyethylene bottle.
7.9 Polyethylene beaker. 100 ml.
7.10 Balance. The sensitivity is 0.01 g.
7.11 Analytical balance. The sensitivity is 0.1 mg.
7.12 Experimental sieve. 0.15 mm in diameter (100 mesh).
7.13 Common instruments and equipment used in general laboratories.
8 samples
8.1 Sample collection and preservation Solid waste samples were collected in accordance with the relevant regulations of HJ/T 20 and HJ/T 298. The collected sample is in the sampling bottle Sealed in (7.8).
8.2 Preparation of samples
8.2.1 Preparation of solid or dry semi-solid samples Accurately weigh 10 g (m1, accurate to 0.01 g) sample, air dry or freeze dry, weigh again (m2, accurate to 0.01 g), ground, all sieved (7.12), ready for use.
8.2.2 Preparation of semi-solid samples in liquid or without drying A sample of 1 g to 10 g (m1, accurate to 0.01 g) was weighed directly into nickel ruthenium (7.7).
8.3 Preparation of samples
8.3.1 Preparation of solid or dry semi-solid samples
8.3.1.1 Weigh 0.10 g~0.25 g (m3, accurate to 0.1 mg) of the dried sieved sample (8.2.1) and place it in advance.
Add appropriate amount of sodium hydroxide (7.7) in the bottom of sodium hydroxide (6.2). 3 g of sodium hydroxide (6.2) is evenly covered on the sample table the surface was capped, placed in a muffle furnace (7.4), and subjected to alkali fusion digestion according to the heating procedure of Table 1.
8.3.1.2 After digestion, wait until the temperature drops to room temperature, remove the nickel crucible, and divide it with about 80 ml of hot water (about 80 ° C ~ 90 ° C).
The secondary leaching was carried out in a polyethylene beaker (7.9). If necessary, use hot plate (7.5) or ultrasonic cleaner (7.6) Auxiliary dissolution. Slowly add 5 ml of hydrochloric acid solution (6.9), transfer to 100 ml of the colorimetric tube after cooling.
Dilute the water to the mark, shake it, let it stand or filter it with a qualitative filter paper (6.14).
Table 1 Solid waste alkaline melting digestion temperature program
Heating step alkali melting temperature (°C) holding time (min)
48.3.2 Preparation of semi-solid samples in liquid or without drying
The pH of the sample (8.2.2) was adjusted to 11 to 12 with a sodium hydroxide solution (6.7) and placed on a hot plate (7.5).
Set the temperature from 120 ° C to 150 ° C, evaporate to dryness in a fume hood, cool to room temperature, add 3 g of sodium hydroxide (6.2) Prepare according to the procedure of 8.3.1.2.
8.4 Preparation of blank samples Without the sample, the preparation of the blank sample was carried out in the same manner as in the preparation of the sample (8.3).
9 Analysis steps
9.1 Establishment of the standard curve Accurately remove 0.10 ml, 0.50 ml, 1.00 ml, 2.00 ml, 5.00 ml, 10.0 ml of fluoride standard solution (6.12) in 6 50 ml plug color tubes, add 15 ml total ionic strength adjustment buffer solution (6.10) and dilute to the standard with water.
Line, mix. The standard series fluoride ion concentration is 0.10mg/L, 0.50mg/L, 1.00 mg/L, 2.00 mg/L, 5.00 mg/L and 10.0 mg/L.
Pour the solution into a polyethylene beaker (7.9), carefully stir to avoid eddy currents, insert the electrode (7.2), press fluorine the ion concentration was measured in order from low to high. The instrument reading is stable (the electrode potential response value fluctuates no more than 0.2) mV/min), the potential response value 1E (mV) was recorded. Taking the logarithm of the fluoride ion mass concentration as the abscissa, corresponding to the potential response value is the ordinate and a standard curve is established.
9.2 Sample determination Accurately absorb the supernatant of the sample to be tested (8.3) or the filtered solution 10.0 ml in a 50 ml colorimetric tube, add 1~ 2 drops of bromocresol purple indicator (6.13), shake well, add hydrochloric acid solution (6.9) dropwise, shake while shaking until the solution is the blue-violet mutation is yellow, add 15 ml total ionic strength adjustment buffer solution (6.10), dilute to the mark with water, and mix.
The measurement was carried out in the same manner as the establishment of the standard curve (9.1).
Note. If the amount of fluorine in the sample is high, the sampling volume can be appropriately reduced.
9.3 Blank test
Accurately pipette blank sample (8.4) 10.0 ml into a 50 ml colorimetric tube and add 0.1 ml of fluoride standard solution (6.12).
The measurement was carried out in the same manner as in the measurement of the sample (9.2), and the calculated fluorine content was subtracted by 5 µg.
10 Calculation and representation of results
10.1 Calculation of results
10.1.1 Mass concentration of fluorine in the sample the mass concentration of fluorine in the sample is 1 (mg/L), calculated according to formula (1).
1lg E ES
Where. 1 - the mass concentration of fluorine in the sample, mg/L;
1E - potential response of the sample, mV;
E - the intercept of the standard curve, mV;
S - slope of the standard curve, mV.
10.1.2 Solid or dry semi-solid waste the fluorine content w (g/kg) in the sample is calculated according to formula (2).
VV mw m V m
x x= xx x (2)
Where. w -- the content of fluorine in solid waste, g/kg;
1 - the mass concentration of fluorine in the sample, mg/L;
3V - the volumetric volume of the liquid to be tested, ml;
1V - the volumetric volume of the sample after digestion, ml;
3m - the mass of the sample after grinding and sieving, g;
2V -- the volume of the sample taken during the measurement, ml;
2m - the mass of the solid waste sample after drying, g;
1m - mass of solid waste sample weighed, g.
10.1.3 Semi-solid solid waste in liquid or without drying the content of fluorine in the sample w (mg/kg) is calculated according to formula (3).
V Vw m V
x x= x (3)
Where. w -- the content of fluorine in solid waste, mg/kg;
1 - the mass concentration of fluorine in the sample, mg/L;
3V - the volumetric volume of the liquid to be tested, ml;
1V - the volumetric volume of the sample after digestion, ml;
1m - mass of solid waste sample, g;
2V -- The volume of the sample taken during the measurement, ml.
10.2 Results are expressed the retention of the number of digits after the decimal point is consistent with the method detection limit, and up to 3 significant digits are retained.
11 Precision and accuracy
11.1 Precision
6 six laboratories for sewage sludge, electroplating sludge with fluorine content of 0.88 g/kg, 1.17 g/kg and 1.71 g/kg, respectively the six solid waste solid waste samples of the waste fly ash were subjected to six repeated measurements. The relative standard deviations in the laboratory were as follows.
3.2% to 8.3%, 3.5% to 9.8%, 4.9% to 8.4%; the relative standard deviations between laboratories are. 3.8%, 6.8%, 7.4%;
The repeatability limits were. 0.13 g/kg, 0.20 g/kg, 0.28 g/kg; the reproducibility limits were. 0.15 g/kg, 0.29 g/kg, 0.44 g/kg.
Six laboratories conducted six repeated tests on a uniform sample of mixed solid waste liquid solid waste with a fluorine content of 522 mg/kg.
The relative standard deviation in the laboratory is 2.3% to 11%; the relative standard deviation between laboratories is 12%; the repeatability limit is 99.6.
Mg/kg; reproducibility limit is 190 mg/kg.
11.2 Accuracy
Six laboratories have two solid solids for sewage sludge and electroplating sludge with a fluorine content of 0.88 g/kg and 1.17 g/kg.
The unified sample of body waste was tested for spiked recovery. The scalar quantity was 1.00 g/kg and 2.50 g/kg, respectively.
The circumference is 89.0%-94.0% and 90.0%-95.2% respectively; the final recoveries of the spiked recovery are 92.5%±4.2% and 92.7%, respectively.
Six laboratories tested the standard for the recovery of liquid solid waste of mixed acid waste liquid with a fluorine content of 522 mg/kg.
The test was 1.00×103 mg/kg, the recoveries ranged from 81.9% to 91.2%, and the final recovery was 86.3%.
12 Quality Assurance and Quality Control
12.1 Analyze at least 2 laboratory blanks per batch of samples and the results should be less than 1.0 µg.
12.2 A standard curve should be established for each batch of samples. The correlation coefficient of the standard curve is >=0.999. Temperature between 0 ° C ~ 30 ° C when the fluoride ion concentration is changed by 10 times, the absolute value of the electrode potential change should satisfy 54.0 mV to 60.0 mV.
12.3 An intermediate concentration point of a standard curve shall be determined for every 20 samples or batches (less than 20 samples/batch) the relative error between the measurement result and the standard concentration value should be between ±10%. Otherwise, you should find the reason and re-establish the standard curve.
12.4 One parallel sample should be analyzed for every 20 samples or batches (less than 20 samples/batch).
The relative deviation should be <= 30%.
12.5 One matrix spiked sample should be analyzed for every 20 samples or batches (less than 20 samples/batch), spiked recovery should be controlled at 75% to 110%.
13 Waste treatment
The waste generated in the experiment should be collected and stored in a centralized manner, and entrusted by qualified units for processing.
14 Precautions
14.1 When heating a liquid or semi-solid sample that does not require drying, take care to avoid overheating and cause the sample to splash.
714.2 The test solution should be allowed to reach room temperature before the measurement. The standard series and the test solution should be measured at the same temperature and stirring speed.
During the measurement, the temperature change should not exceed ± 2 °C.
14.3 After measuring a sample with a high fluorine content, the electrode should be placed in water and washed to the maximum potential value to prevent the electrode from being generated.
Recall the effect.
......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 7 pages — is available in the English PDF.
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