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HJ 671-2013 English PDF

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HJ 671-2013: Water quality. Determination of total phosphorus. Flow injection Analysis(FIA) and Ammonium molybdate spectrophotometry
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Standard ID	Contents [version]	USD	STEP2	[PDF] delivered in	Standard Title (Description)	Status	PDF
HJ 671-2013	English	289	Add to Cart	3 days [Need to translate]	Water quality. Determination of total phosphorus. Flow injection Analysis(FIA) and Ammonium molybdate spectrophotometry	Valid	HJ 671-2013

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Basic data

Standard ID	HJ 671-2013 (HJ671-2013)
Description (Translated English)	Water quality. Determination of total phosphorus. Flow injection Analysis(FIA) and Ammonium molybdate spectrophotometry
Sector / Industry	Environmental Protection Industry Standard
Classification of Chinese Standard	Z16
Classification of International Standard	13.060
Word Count Estimation	11,160
Quoted Standard	GB 11893; HJ/T 91; HJ/T 164
Regulation (derived from)	Ministry of Environmental Protection Notice No. 63 of 2013
Issuing agency(ies)	Ministry of Ecology and Environment
Summary	This standard specifies the determination of total phosphorus in water flow injection - molybdate spectrophotometry. This standard applies to surface water, groundwater, sewage and industrial effluent total phosphorus determination. When the detection cel

HJ 671-2013: Water quality. Determination of total phosphorus. Flow injection Analysis(FIA) and Ammonium molybdate spectrophotometry

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Water quality.Determination of total phosphorus.Flow injection Analysis(FIA) and Ammonium molybdate spectrophotometry National Environmental Protection Standard of the People's Republic Determination of total phosphorus in water Flow injection-ammonium molybdate spectrophotometry Water quality-Determination of total phosphorus-Flow injection Analysis (FIA) and Ammonium molybdate spectrophotometry Published on.2013-10-25 2014-01-01 implementation Ministry of Environmental Protection released

Content

Preface II 1 Scope..1 2 Normative references..1 3 method principle..1 4 interference and elimination. 2 5 reagents and materials. 2 7 samples.4 8 Analysis steps..4 9 result calculation and representation..4 10 Precision and Accuracy 5 11 Quality Assurance and Quality Control.5 12 Notes 6

Foreword

To implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on Water Pollution Prevention and Control, to protect the environment, This standard is formulated to ensure human health and standardize monitoring methods for total phosphorus in water. This standard specifies a flow injection-ammonium molybdate spectrophotometric method for the determination of total phosphorus in water. This standard is the first release. This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection. This standard is mainly drafted by. Suzhou Environmental Monitoring Center Station and Changshu Environmental Monitoring Station. This standard is verified by. Beijing Environmental Protection Monitoring Center, Nantong Environmental Monitoring Center Station, Jiangsu Marine Fisheries Institute, Suzhou Water Supply Company Water Quality Testing Center, Nanchang Environmental Monitoring Station and Changshu Environmental Monitoring Station. This standard was approved by the Ministry of Environmental Protection on October 25,.2014. This standard has been implemented since January 1,.2014. This standard is explained by the Ministry of Environmental Protection. Water quality - Determination of total phosphorus - Flow injection - Ammonium molybdate spectrophotometric method

1 Scope of application

This standard specifies a flow injection-ammonium molybdate spectrophotometric method for the determination of total phosphorus in water. This standard applies to the determination of total phosphorus in surface water, groundwater, domestic sewage and industrial wastewater. When the detection cell optical path is 10mm, the detection limit of this method is 0.005mg/L (in P), and the measurement range is 0.020 mg/L. ~1.00mg/L.

2 Normative references

The contents of this standard refer to the terms in the following documents. For undated references, the valid version applies to This standard. GB 11893 Determination of total phosphorus in water - Ammonium molybdate spectrophotometric method HJ/T 91 Surface Water and Wastewater Monitoring Technical Specifications HJ/T 164 Technical Specifications for Groundwater Environmental Monitoring

3 Principle of the method

3.1 Working principle of flow injection analyzer In a closed pipeline, a volume of sample is injected into a continuous flow of carrier liquid, and the sample and reagent are in a chemical reaction module. Mix and react in a specific order and ratio, and enter the flow detection cell for photometric detection under incomplete reaction conditions. 3.2 Principles of chemical reactions Under acidic conditions, various forms of phosphorus in the sample are hydrolyzed by high temperature and high pressure at 125 ° C, and then mixed with potassium persulfate solution. UV digestion, all of which is oxidized to orthophosphate. Under the catalysis of cerium salt, orthophosphate reacts with ammonium molybdate to form heteropolyphosphate acid. The compound was reduced by ascorbic acid to form a blue complex, and the absorbance was measured at a wavelength of 880 nm. Refer to the work flow chart, as shown in Figure 1. 1-peristaltic pump 2 - heating tank (125 ° C) 3-UV digestion device (UV254nm) 4-excluding bubbles 5-injection valve 6-reaction (mixing) ring 7-detection cell 10mm 880nm S-sample R1-sulfuric acid solution I (5.13) R2-potassium persulfate digestion solution (5.15) R3-developer (5.18) R4-reducing agent (5.19) C-sulfuric acid carrier liquid (5.20) W-waste liquid Fig.1 Flow chart of flow injection-ammonium molybdate spectrophotometric determination of total phosphorus

4 interference and elimination

4.1 The arsenic, chromium and sulfur in the sample interfere with the determination of total phosphorus. For the specific elimination method, see GB 11893. 4.2 The turbidity or chromaticity interference of the sample can be corrected by the compensation measurement. Specific elimination method. using chroma-turbidity compensation solution (5.28) Replace the molybdate developer (5.18), analyze the sample, and measure the correction value. Sample measurement minus subtraction Value, the corrected measurement is obtained. 4.3 When the pH of the sample is < 2, there will be a refractive indication (referring to a small negative peak in front of the analyte peak) or a double peak Disturbance; when the pH of the sample is >10, it will cause positive interference to the measurement. Therefore, when the sample pH < 2 or > 10, it should be before analysis The pH of the sample was adjusted to neutral.

5 reagents and materials

Unless otherwise stated, analytically pure reagents that meet national standards were used for the analysis. Experimental water is freshly prepared and conductance Deionized water having a rate of less than 0.5 μS/cm (25 ° C). In addition to the standard solution, other solutions and experimental water are used with helium (5.30) Or ultrasonic (6.3) degassing. 5.1 Sulfuric acid. ρ (H2SO4) = 1.84 g/ml. 5.2 Potassium persulfate (K2S2O8). 5.3 Ammonium molybdate [(NH4) 6Mo7O24·4H2O]. 5.4 Potassium bismuth tartrate [K(SbO) C4H4O6·1⁄2H20]. 5.5 sodium hydroxide (NaOH). 5.6 Ascorbic acid (C6H8O6). 5.7 sodium lauryl sulfate (NaC12H25SO4). 5.8 Sodium chloride (NaCl). 5.9 Potassium dihydrogen phosphate (KH2PO4). excellent grade, dry constant weight at 105 °C ± 5 °C, stored in a desiccator. 5.10 Sodium pyrophosphate (Na4P2O7·10H2O). sealed and stored. 5.11 Pyridoxal 5-phosphate (C8H10NO6P·H2O). purity greater than 95%. Store at 2 ° C ~ 8 ° C sealed. 5.12 Tetrasodium edetate (Na4EDTA, C10H12O8N2Na4). 5.13 Sulfuric acid solution I.c(H2SO4)=2 mol/L 106.5 ml of sulfuric acid (5.1) was slowly added to 800 ml of water, and after cooling, it was diluted with water to 1000 ml. 5.14 sulfuric acid solution II. c (H2SO4) = 0.028 mol/L 1.5 ml of sulfuric acid (5.1) was added to 1000 ml of water. 5.15 potassium persulfate digestion solution 26 g of potassium persulfate (5.2) was added to 800 ml of water, dissolved, and diluted to 1000 ml with water and mixed. The solution at room temperature Stored in the dark for 1 month. 5.16 Ammonium molybdate solution Weigh 40.0g ammonium molybdate (5.3) dissolved in 800ml water, dissolve it, dilute it with water to 1000ml and mix it, store it in poly In the vinyl bottle. The solution was stored at 4 ° C and was stable for 2 months. 5.17 Potassium tartrate storage solution Weigh 3.0g of bismuth potassium tartrate (5.4) dissolved in 800ml of water, dissolve, dilute with water to 1000ml and mix, store In dark polyethylene bottles. The solution was stored at 4 ° C and was stable for 2 months. 5.18 chromogenic agent Add 213ml ammonium molybdate solution (5.16) and 72ml potassium bismuth tartrate solution (5.17) to about 500ml of water, plus Add 22.8 g of sodium hydroxide (5.5), dissolve and dilute to 1000 ml with water and mix. The solution is stored at 4 ° C and is stable 1 Months. 5.19 reducing agent Weigh 70.0g of ascorbic acid (5.6) dissolved in 800ml of water, then add 1.0g of sodium lauryl sulfate (5.7) to dissolve Dilute to 1000 ml with water and mix. The solution was stored at 4 ° C and was stable for 2 weeks. 5.20 sulfuric acid carrier liquid 40 ml of sulfuric acid (5.1) was slowly added to 800 ml of water. After cooling, add 5g sodium chloride (5.8) and 1.0g twelve Sodium alkyl sulfate (5.7), diluted to 1000 ml with water and mixed. The solution is stable for 1 week. 5.21 Standard stock solution of potassium dihydrogen phosphate. ρ(P)=1000mg/L Weigh 4.394g potassium dihydrogen phosphate (5.9) dissolved in water, dissolved and transferred to a 1000ml volumetric flask, add 2.5ml Sulfuric acid (5.1), make up to volume with water and mix. Stored in stoppered glass bottles, the solution is stored at 4 ° C for 6 months. Or buy a commercially available certified standard solution directly. 5.22 Potassium dihydrogen phosphate standard use solution I. ρ (P) =10.00 mg/L The appropriate amount of potassium dihydrogen phosphate standard stock solution (5.21) was weighed and prepared by dilution with water. The solution can be stored at 4 ° C Months. 5.23 Potassium dihydrogen phosphate standard use solution II. ρ (P) = 0.50 mg/L The appropriate amount of potassium dihydrogen phosphate standard stock solution (5.21) was weighed and prepared by dilution with water. Available at the time of use. Note. If the sample is fixed with sulfuric acid (5.1), the standard solution also needs to be prepared with a sulfuric acid matrix, ie with a sulfuric acid solution (5.14). Prepare a standard solution for water. 5.24 Standard stock solution of sodium pyrophosphate. ρ(P) = 500mg/L Weigh 3.600g of sodium pyrophosphate (5.10) dissolved in water, transfer it to a 1000ml volumetric flask, dilute to volume with water and mix. The solution The solution is stored in a sealed container at 4 ° C for 3 months. 5.25 Standard use solution of sodium pyrophosphate. ρ(P) =0.50mg/L Take an appropriate amount of sodium pyrophosphate standard stock solution (5.24) and prepare it by dilution with water. The solution was stable for 1 week at 4 °C. 5.26 standard stock solution of pyridoxal 5-phosphate. ρ(P) =500mg/L Weigh 0.8561g (100% by purity) pyridoxal 5-phosphate (5.11) dissolved in an appropriate amount of water and transferred to.200ml capacity In a measuring flask, make up to volume with water and mix in a brown stoppered glass bottle. The solution can be stored for 3 months at 4 °C. 5.27 Standard use solution of pyridoxal 5-phosphate. ρ(P) =0.50mg/L The appropriate amount of pyridoxal 5-phosphate standard stock solution (5.26) was weighed and prepared by dilution with water. Available at the time of use. 5.28 Chroma turbidity compensation fluid Add 72ml of potassium bismuth tartrate stock solution (5.17) to about 500ml of water, then add 22.8g of sodium hydroxide (5.5). After dissolution, it was diluted with water to 1000 ml. The solution is stable for 1 week. 5.29 NaOH-EDTA cleaning solution 65 g of sodium hydroxide (5.5) and 6 g of tetrasodium ethylenediaminetetraacetate (5.12) were weighed and dissolved in 1000 ml of water. 5.30 Helium. Purity ≥99.99%.

6 Instruments and equipment

6.1 Flow injection analyzer. autosampler, chemical analysis unit (ie chemical reaction module, channel. by peristaltic pump, note Into the valve, reaction line, pre-treatment box and other components), detection unit (flow cell detection wavelength 880nm) and data processing yuan. The pretreatment cartridge includes a heating bath and an ultraviolet digestion device. 6.2 Balance. The accuracy is 0.0001g. 6.3 Ultrasonic machine. frequency 40KHz. 6.4 Common instruments and equipment used in general laboratories.

7 samples

Samples were collected and stored in accordance with the relevant regulations of HJ/T 91 and HJ/T 164. Prior to sampling, all vessels in contact with the sample were rinsed with water and the samples were collected in cleaned polyethylene or glass vials. Pick Immediately after the collection, sulfuric acid (5.1) should be added to pH ≤ 2, and it can be stored at room temperature for 24 hours. It can be frozen at -20 °C for 1 month. Note. Samples with less phosphorus (total phosphorus concentration ≤ 0.1mg/L) should not be stored in polyethylene bottles, except for cryopreservation.

8 Analysis steps

8.1 Commissioning of the instrument Install the analysis system, debug the instrument, and set the operating parameters according to the instrument manual. After booting in the order specified by the instrument, Pure water replaces all reagents, checking the tightness of the entire analytical flow path and the smoothness of liquid flow. After the baseline is stable (about At 20 min), the system starts to enter the reagent. After the baseline is stabilized again, 8.2 to 8.4 are performed. 8.2 Calibration 8.2.1 Preparation of the standard series Take appropriate amount of potassium dihydrogen phosphate standard use solution I (5.22), dilute to 100ml with water, prepare 6 Standard series of concentration points. The total phosphorus concentration was 0.000 mg/L, 0.020 mg/L, 0.100 mg/L, 0.200 mg/L, 0.500 mg/L and 1.00 mg/L. 8.2.2 Drawing of the calibration curve Measure the appropriate standard series (8.2.1), respectively, in the sample cup, from the low concentration to the high concentration by the injector Sampling and measurement. Taking the measured signal value (peak area) as the ordinate, the corresponding total phosphorus mass concentration (in P, mg/L) For the abscissa, draw a calibration curve. 8.3 Determination The measurement of the sample was carried out under the same conditions as in the drawing of the calibration curve. Note. If the total phosphorus content of the sample exceeds the calibration curve range, the appropriate amount of sample should be diluted and measured on the machine. 8.4 Blank test Replace the sample with an appropriate amount of experimental water and perform a blank test in accordance with step 8.3.

9 Calculation and representation of results

9.1 Calculation of results The mass concentration of total phosphorus (in terms of P, mg/L) in the sample was calculated according to formula (1). Yaf ρ −= × (1) In the formula. Ρ--the mass concentration of total phosphorus in the sample, mg/L; y -- determine the signal value (peak area); a -- the intercept of the calibration curve equation; b -- the slope of the calibration curve equation; f -- dilution factor. 9.2 Results representation When the measurement result is less than 1.00 mg/L, the measurement result is retained to three decimal places; when it is greater than or equal to 1.00 mg/L, The measurement results retain three significant figures. 10 Precision and accuracy 10.1 Precision Six laboratories tested the uniform samples with total phosphorus concentrations of 0.020 mg/L, 0.215 mg/L, and 1.58 mg/L, respectively. The relative standard deviations in the experimental room were 1.9%~5.8%, 0.3%~3.0%, 0.3%~1.0%, respectively; the relative standard deviation between laboratories Respectively 9.5%, 2.8%, 1.2%; repeatability limits. 0.003 mg/L, 0.009 mg/L, 0.032 mg/L; reproducibility The limits are. 0.006 mg/L, 0.018 mg/L, and 0.062 mg/L. 10.2 Accuracy 6 laboratories have certified standards for total phosphorus concentrations of 0.215 mg/L ± 0.012 mg/L and 1.58 mg/L ± 0.06 mg/L, respectively. For the determination of the substance, the relative errors are. 0.0%~4.2%, 0.0%~2.5%; the relative error final values are. 2.1%±4.0%, 1.4% ± 1.9%. The total concentration of phosphorus in the six laboratories was 0.031mg/L~0.172mg/L, 0.146mg/L~0.680mg/L and 0.257 respectively. Three different types of actual samples (surface water, domestic sewage, industrial wastewater) of mg/L~1.20 mg/L were spiked and recovered. The recoveries of the spiked samples were. 90.0%~108%, 95.5%~108%, 92.3%~108%; the final value of the spiked recovery rate Do not. 99.3% ± 11.8%, 103% ± 9.4%, 99.1% ± 11.4%. 11 Quality Assurance and Quality Control 11.1 Blank test At least 2 blank samples shall be measured for each batch of samples, and the blank value shall not exceed the method detection limit. Otherwise, you should find out the reason and re The sample can only be determined after analysis until it is qualified. 11.2 Calibration validity check A calibration curve must be drawn for each batch of samples. The correlation coefficient of the calibration curve is γ ≥ 0.995. For each sample analyzed, a calibration curve intermediate concentration solution is used for calibration verification, and the measurement results are relatively biased. The difference should be ≤ 5%, otherwise the calibration curve should be redrawn. 11.3 Precision Control At least 10% of the parallel samples should be determined for each batch of samples. When the number of samples is less than 10, at least one parallel sample should be determined. When the total phosphorus concentration is ≤0.02mg/L, the relative deviation of the parallel sample is ≤25%; when the total phosphorus concentration is >0.02mg/L, the relative of the parallel sample The deviation is ≤10%. 11.4 Accuracy Control At least 10% of the spiked sample shall be determined for each batch of samples. When the number of samples is less than 10, at least one spiked sample shall be determined. The spiked recovery rate should be between 80% and 120%. If necessary, each batch of samples shall have at least one known quality control sample, and the test results shall be in the uncertainty given by it. Inside. 11.5 System Performance Check Regularly use the sodium pyrophosphate standard use solution (5.25) to verify the hydrolysis efficiency of the method, using the pyridoxal 5-phosphate standard to dissolve The digestion efficiency of the liquid (5.27) verification method is generally 1 time in 2 weeks. Calibrate the system (8.2) first, then parallel analysis of sodium pyrophosphate standard use solution (5.25) or pyridoxal 5-phosphate Calculate the hydrolysis or digestion efficiency R,R according to formula (2) using solution (5.27) and potassium dihydrogen phosphate standard solution (5.23). Should be greater than 90%. 100%R ρρ= × (2) In the formula. R--hydrolysis or digestion efficiency, %; ρ1--Sodium pyrophosphate standard use solution (5.25) or pyridoxal 5-phosphate standard use solution (5.27), mg/L; The measurement result of the standard use solution of ρ2--potassium dihydrogen phosphate (5.23), mg/L. Note. When the measured result of the certified reference material is lower than the lower limit of its uncertainty range, 11.5 is required. 12 Precautions 12.1 Because the flow path of the flow injection analyzer is small, it is not suitable for determining more particulate matter or larger particle size than suspended particles. 250 μm sample. 12.2 Reagent and ambient temperature influence analysis results, the reagents stored in the refrigerator should be placed at room temperature (20 ± 5 ° C) before use. The room temperature fluctuation during the analysis cannot exceed ± 2 °C. 12.3 To reduce baseline noise, the reagents should be kept clear and filtered if necessary. Closed chemical reaction system will dry if there are bubbles Disturbance measurement, therefore, all solutions except the standard solution must be degassed, degassing with helium for 1 min or ultrasonic degassing for 30 min. 12.4 After each analysis, clean the analytical pipeline with pure water and remove the filter from the flow detection tank in time. Into the dryer, dust and moisture. 12.5 Pre-treatment box heaters When the heating temperature is close to 80 °C, it should ensure that there is liquid flow in the heater's pipeline. 12.6 Different types of flow analyzers can be selected with reference to this standard to select the appropriate instrument conditions.

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