HJ 1075-2019 English PDF

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HJ 1075-2019: Water quality--Determination of turbidity--Nephelometry
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Basic data

Standard ID: HJ 1075-2019 (HJ1075-2019)
Description (Translated English): Water quality--Determination of turbidity--Nephelometry
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z16
Classification of International Standard: 13.060
Word Count Estimation: 12,162
Date of Issue: 2019
Date of Implementation: 2020-06-30
Issuing agency(ies): Ministry of Ecology and Environment

HJ 1075-2019: Water quality--Determination of turbidity--Nephelometry

---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.
Water quality--Determination of turbidity--Nephelometry National Environmental Protection Standard of the People's Republic of China HJ 1076-2019 Ambient air ammonia, methylamine, dimethylamine and trimethylamine Determination of ion chromatography Ambient air-Determination of ammonia, methylamine, dimethylamine and trimethylamine-Ion chromatography 2019-12-31 released 2020-06-30 implementation Released by the Ministry of Ecology and Environment

Contents

Foreword ... ii 1 Scope ... 1 2 Normative references ... 1 3 Methodology ... 1 5 Reagents and materials ... 1 6 Instruments and equipment ... 1 7 Sample ... 3 8 Analysis steps ... 4 9 Results calculation and representation ... 5 10 Precision and accuracy ... 5 11 Quality Assurance and Quality Control ... 6 12 Notes ... 6 Appendix A (Informative) Summary of Methods Precision and Accuracy ... 7

Foreword

In order to implement the "Environmental Protection Law of the People's Republic of China" Environment, protect human health, standardize the determination methods of ammonia, methylamine, dimethylamine and trimethylamine in ambient air quasi. This standard specifies the determination of ammonia, methylamine, dimethylamine, and Ion chromatography of trimethylamine. Appendix A of this standard is an informative appendix. This standard is issued for the first time. This standard is formulated by the Department of Eco-Environmental Monitoring, Laws and Standards Department of the Ministry of Ecology and Environment. This standard was drafted. Dalian Ecological Environment Monitoring Center, Liaoning Province. This standard is verified by. Shenyang Eco-environment Monitoring Center, Liaoning Province, Anshan Eco-Environment Monitoring Center, Liaoning Province, Chengdu Municipal Environmental Monitoring Center Station, Tianjin Ecological Environment Monitoring Center, Jilin City Environmental Monitoring Station, Xiamen City Environmental Monitoring Station, Jiangxi Yangzhou Environmental Monitoring Center of Jiangsu Province and Environmental Monitoring Center Station of Inner Mongolia Autonomous Region. This standard was approved by the Ministry of Ecology and Environment on December 31,.2019. This standard will be implemented from June 30, 2020. This standard is explained by the Ministry of Ecology and Environment. Ambient air. Determination of ammonia, methylamine, dimethylamine and trimethylamine. Ion chromatography Warning. The solvents and reagents used in the experiment are strongly corrosive and irritating. The reagent preparation process should be ventilated. Carry out in the cabinet; wear protective equipment as required to avoid inhalation and contact with skin and clothing.

1 Scope

This standard specifies ion chromatography for the determination of ammonia, methylamine, dimethylamine and trimethylamine in ambient air. This standard applies to ammonia, methylamine, dimethylamine and trimethylammonium in the air of ambient air and fixed pollution source fugitive emission monitoring points. Determination of amines. When the ambient air sampling volume is 30 L and the absorption volume is 10 ml, this standard ammonia, methylamine, dimethylamine and trimethylamine The detection limits are 0.003 mg/m3, 0.009 mg/m3, 0.009 mg/m3, and 0.007 mg/m3, and the lower detection limits are 0.012 mg/m3, 0.036 mg/m3, 0.036 mg/m3, and 0.028 mg/m3.

2 Normative references

This standard refers to the following documents or clauses therein. For undated references, the valid version applies to this standard. HJ 194 Technical Specifications for Manual Monitoring of Ambient Air Quality HJ/T 55 Technical guidelines for fugitive emissions monitoring of air pollutants

3 Method principle

Ambient air samples are filtered through a filter membrane. After the target compound is absorbed by the dilute sulfuric acid absorption solution, the cation chromatography column is used to exchange the analytes. Ionization, conductance detector detection, qualitative retention time, external standard method.

4 Reagents and materials

Unless otherwise specified, analytical reagents that comply with national standards are used in the analysis, and the experimental water is freshly prepared ammonia-free water. 4.1 Sulfuric acid. ρ (H2SO4) = 1.84 g/ml. 4.2 Nitric acid (HNO3). excellent grade pure. 4.3 Methanesulfonic acid. w (CH3SO3H) ≥99%. 4.4 Ammonium chloride (NH4Cl). excellent grade pure. 4.5 Methylamine hydrochloride (CH5N · HCl). 98.0%. 4.6 Dimethylamine hydrochloride (C2H7N · HCl). 99.0%. 4.7 Trimethylamine hydrochloride (C3H9N · HCl). 98.0%. 4.8 Sulfuric acid absorption solution. c (1/2H2SO4) = 0.01 mol/L. Measure 2.7 ml of sulfuric acid (4.1), dilute with water to 1000 ml, and mix to prepare a 0.1 mol/L sulfuric acid solution. Before use When diluted with water 10 times. 4.9 Ammonia standard stock solution. ρ (NH3) = 500 mg/L. Weigh 0.3928 g of ammonium chloride (4.4) and dissolve it in water, then transfer it to a 250 ml volumetric flask and dilute it to the mark with water. Mix well. Stored in polyethylene bottles, refrigerated below 4 ° C, protected from light and sealed for up to three months. Can also be purchased with a commercial license standard material. 4.10 Methylamine standard stock solution. ρ (CH5N) = 500 mg/L. Weigh 0.2772 g of methylamine hydrochloride (4.5) in water, transfer to a 250 ml volumetric flask, and dilute to the mark with water. Shake well, store in a polyethylene bottle, refrigerate below 4 ° C, protect from light and seal for three months. You can also buy a commercially available certificate Quasi-substance. 4.11 Dimethylamine standard stock solution. ρ (C2H7N) = 500 mg/L. Weigh 0.2284 g of dimethylamine hydrochloride (4.6) in water, transfer to a 250 ml volumetric flask, and dilute with water to the standard Line, shake well, store in polyethylene bottle, refrigerate below 4 ℃, protect from light and seal for three months. Can also be purchased with a commercial license standard material. 4.12 Trimethylamine standard stock solution. ρ (C3H9N) = 500 mg/L. Weigh 0.2063 g of trimethylamine hydrochloride (4.7) to dissolve in water, transfer to a 250 ml volumetric flask, and dilute with water to the standard Line, shake well, store in a polyethylene bottle, refrigerate below 4 ° C, protect from light and seal for three months. Commercially available Certified reference materials. 4.13 Mixed Standard Use Solution According to the measured ion concentration range and detection sensitivity, the standard use solution can be prepared. Pipette 5.00 ml ammonia standards separately Stock solution (4.9), 20.0 ml standard methylamine stock solution (4.10), 20.0 ml standard dimethylamine stock solution (4.11), and 20.0 ml Trimethylamine standard stock solution (4.12) was placed in a 250 ml volumetric flask, diluted with water to make it to the mark, and mixed. Formulated to contain A mixed standard of 10.0 mg/L ammonia, 40.0 mg/L methylamine, 40.0 mg/L dimethylamine, and 40.0 mg/L trimethylamine makes the standard With liquid. Stored in polyethylene bottles, refrigerated, protected from light and sealed at 4 ° C or lower for one month. 4.14 Stock solution of methanesulfonic acid. c (CH3SO3H) = 1 mol/L. Pipette 32.0 ml of methanesulfonic acid (4.3) into an appropriate amount of water, then transfer to a 500 ml volumetric flask and dilute with water to the standard Line and mix. Stored in polyethylene plastic bottles, refrigerated below 4 ° C, and stored in the dark for two years. 4.15 Use solution of methanesulfonic acid. c (CH3SO3H) = 22 mmol/L. Pipette 44.0 ml of mesylate eluent stock solution (4.14) into a.2000 ml volumetric flask, dilute with water to the mark, and mix. Provisional use. 4.16 Nitric acid eluent. c (HNO3) = 4.6 mmol/L. Transfer 0.294 ml 70% nitric acid (4.2) into a 1000 ml volumetric flask, dilute with water to the mark, mix well, and use immediately Match. 4.17 Filter. 0.45 μm. 4.18 Microporous membrane. 0.22 μm, polyethersulfone or equivalent.

5 Instruments and equipment

5.1 Air sampler. flow range, (0 ～ 1) L/min, equipped with thermal insulation device and filter clamp. 5.2 Ion chromatograph. equipped with a conductivity detector. 5.3 Column. 5.3.1 Suppressed chromatographic column. the packing is polystyrene-divinylbenzene copolymer, a separation column with carboxylic acid functional groups, 5.5 μm diameter, 5 mm inner diameter, 250 mm column length or other equivalent high capacity column. 5.3.2 Non-suppressive chromatographic column. The packing is a separation column with carboxyl silica gel functional group, the particle size is 5 μm, the inner diameter is 4.0 mm, The column is 250 mm long and has a pH tolerance range of 2 to 7 or other equivalent high capacity columns. 5.4 Colorimetric tube with stopper. 10 ml. 5.5 Multiwell glass absorption tube. 10 ml. 5.6 General laboratory instruments and equipment.

6 samples

6.1 Sample collection and storage 6.1.1 Collection of samples The layout and sampling of air in ambient air and fugitive emission monitoring points of fixed pollution sources should comply with HJ 194 and Relevant regulations in HJ/T 55. Before sampling, air tightness check and flow calibration should be performed on the sampler, and the suction pump should be turned on to Pump down at a flow rate of 0.5 L/min for about 5 minutes to replace the air in the sampling system. When sampling, place the filter (4.17) in the filter holder and connect it to a porous glass plate containing 10.0 ml of sulfuric acid absorption solution. Tube (5.5), connected to the air sampler (5.1) with a silicone tube, and collected ambient air samples at a flow rate of 0.5 L/min for 60 min. When the actual concentration is higher than the upper limit of the curve, appropriately reduce the sampling flow or shorten the sampling time, and record the sampling temperature and atmosphere at the same time Parameters such as pressure. Each sampling should bring at least one full-program blank sample, and bring the porous glass plate absorbent tube (5.5) prepared in the same batch with Go to the sampling site, open the two ends, connect with the sampler, immediately remove and close both ends, follow the transportation and storage with the sample (6.1.2) Bring the same conditions back to the laboratory. 6.1.2 Transport and storage of samples After the sample is collected, the air inlet and air outlet of the porous glass plate absorption tube (5.5) are closed with a silicone tube and placed upright in a clean Transport and storage in containers. If it can not be measured in time, the samples should be refrigerated, protected from light and sealed at below 4 ° C, and should be stored within 7 days. 成 analysis. 6.2 Preparation of test specimens Transfer the entire sample (6.1.1) into a 10 ml stopper colorimetric tube (5.4), rinse the absorber tube with an appropriate amount of water and transfer In the colorimetric tube (5.4), make up to the mark and shake well. Filter through a microporous membrane (4.18), discard 2 ml of the initial solution, and collect The filtrate was transferred to a 5 ml stoppered vial for testing. 6.3 Preparation of laboratory blank samples Replace the sample with the same batch and the same volume of sulfuric acid absorption solution (4.8), and prepare according to the sample preparation step (6.2) Laboratory blank sample.

7 Analysis steps

7.1 Reference conditions for ion chromatography 7.1.1 Reference condition 1 (suppressed) Methanesulfonic acid eluent concentration. 22 mmol/L; Column temperature. 40 ° C; Injection volume. 25 μl; Flow rate. 1.0 ml/min. 7.1.2 Reference condition 2 (non-suppressed) Nitrate eluent concentration. 4.6 mmol/L; Column temperature. 35 ° C; Injection volume. 50 μl; Flow rate. 1.0 ml/min. 7.2 Establishment of standard curve Establish a five-point standard curve covering the concentration range of the sample 1. From low concentration to high concentration, transfer to the ion chromatography. When using suppressed ion chromatography, select a suppressed color The column (5.3.1) is analyzed and determined according to the reference conditions of ion chromatography (7.1.1); when non-suppressed ion chromatography is used, Select a non-suppressive column (5.3.2) for analysis and determination in accordance with the reference conditions for ion chromatography (7.1.2). Dissolved in standard series The concentration (mg/L) of the target compound in the liquid is the abscissa, and the peak height or the area is the ordinate. Ammonia, methylamine, diamine Methylamine and trimethylamine calibration curves. Under the ion chromatography conditions specified in this standard, the standard chromatogram of the target compound is shown in Figure 1. And Figure 2. Table 1 Standard series concentrations of target compounds Serial number Standard series concentration (mg/L) Carbamate dimethylamine trimethylamine 1 0.025 0.10 0.10 0.10 2 0.05 0.20 0.20 0.20 3 0.25 1.00 1.00 1.00 4 1.00 4.00 4.00 4.00 5 5.00 20.0 20.0 20.0 1-Ammonia; 2-methylamine; 3-dimethylamine; 4-trimethylamine. Figure 1 Standard chromatogram (suppressed) 1-Ammonia; 2-methylamine; 3-dimethylamine; 4-trimethylamine. Figure 2 Standard chromatogram (non-suppressed) 7.3 Sample determination The measurement of the sample (6.2) was performed according to the same procedure as the standard curve establishment (7.2) and the conditions of ion chromatography. 7.4 Blank test Follow the same procedure as the sample measurement (7.3) and the ion chromatography conditions to measure the laboratory blank sample (6.3).

8 Results calculation and representation

8.1 Calculation of results The volume mass concentration of ammonia, methylamine, dimethylamine and trimethylamine in the air is calculated according to formula (1). nV 0.101 × = ρρ (1) In the formula. ρ-the concentration of the target in the sample, mg/m3; ρ1-target substance concentration in the sample, mg/L; 10.0--absorbent volume, ml; Vn--under standard state (273.15 K, 1013.25 hPa) or reference state (298.15 K, 1013.25 hPa) Sampling volume, L. 8.2 Results representation The number of digits after the decimal point of the measurement result is consistent with the detection limit, and a maximum of three significant digits are retained.

9 Precision and accuracy

9.1 Precision Eight laboratories separately performed uniform actual samples (ammonia, methylamine, and dimethylamine) The actual sample concentrations of trimethylamine and trimethylamine were 1.11 mg/m3, 1.72 mg/m3, 1.75 mg/m3, and 2.39 mg/m3; Low concentration actual sample concentrations were 0.278 mg/m3, 0.104 mg/m3, 0.105 mg/m3, and 0.169 mg/m3 respectively. Six repeated determinations, the relative standard deviations in the laboratory were 0.3% to 4.8% and 0.5% to 6.4%, respectively. The standard deviations are 1.6% to 5.2% and 3.7% to 5.4%, and the repeatability limits are 0.11 mg/m3 to 0.18 mg/m3 and 0.02, respectively. mg/m3 to 0.03 mg/m3, with reproducibility limits of 0.14 mg/m3 to 0.27 mg/m3 and 0.02 mg/m3 to 0.05 mg/m3, respectively. 9.2 Accuracy Eight laboratories separately performed uniform actual samples (ammonia, methylamine, and dimethylamine) And trimethylamine The actual sample concentrations are 0.507 mg/m3, 0 mg/m3, 0 mg/m3, 0.777 mg/m3, respectively; low The actual sample concentrations were 0.096 mg/m3, 0 mg/m3, 0 mg/m3, and 0.076 mg/m3, respectively. Assay, the spiked amounts of ammonia, methylamine, dimethylamine and trimethylamine were 0.667 mg/m3, 1.67 mg/m3, 1.67 mg/m3, and 1.67, respectively. mg/m3 and 0.2 mg/m3, 0.1 mg/m3, 0.1 mg/m3, 0.1 mg/m3. Target compound recovery was 86.7% ～ 110% and 85.8% ～ 114%, the final recoveries are 91.2% ± 8.6% ～ 105% ± 6.0% and 90.9% ± 13.0% ~ 105% ± 9.6%. 10 Quality Assurance and Quality Control 10.1 The correlation coefficient of the standard curve shall be ≥0.995. 10.2 Make at least one laboratory blank and full program blank for each batch of samples. The measurement results should be below the method detection limit. 10.3 Every 20 samples or each batch (less than 20 samples/batch) shall be calibrated once with the middle concentration point of the calibration curve. Quasi-check, the relative error of the standard check should be ≤10%, otherwise the cause should be found and the calibration curve should be redrawn. 10.4 A blank spiked sample should be made for each batch of samples, and the spiked recovery rate should be between 75% and 120%. 11 matters needing attention 11.1 Experimental equipment and experimental environment shall be protected from ammonia pollution. 11.2 The acidity of the actual sample will affect the service life of the column. A column with a large capacity and good acid resistance should be selected. When the sample concentration is high, it can be appropriately diluted to protect the life of the column. 12 Waste treatment The waste generated during the experiment should be collected separately and stored in a centralized manner, safely processed as required or entrusted to a qualified unit for disposal.

Appendix A

(Informative appendix) Summary table of method precision and accuracy Table A.1 Summary of method precision Name CAS number Actual sample concentration Degree (mg/m3) Relative standards in the laboratory Quasi deviation (%) Interlaboratory relative standard Quasi deviation (%) Repeatability limit (Mg/m3) Limit of reproducibility (Mg/m3) Ammonia 7664-41-7 1.11 0.3 ～ 4.8 5.2 0.11 0.19 0.278 0.5 ～ 4.8 5.4 0.03 0.05 Methylamine 74-89-5 1.72 0.3 ～ 3.4 1.6 0.13 0.14 0.104 1.5 ～ 5.5 4.9 0.02 0.02 Dimethylamine 1.75 0.5 ～ 4.2 2.9 0.15 0.20 0.105 1.8 ～ 6.4 4.6 0.02 0.02 Trimethylamine 2.39 0.6 ～ 3.3 3.1 0.18 0.27 0.169 1.8 ～ 5.2 3.7 0.02 0.03 Table A.2 Summary of method accuracy Name CAS number Spiked concentration (Mg/m3) Actual sample concentration (Mg/m3) After the actual sample is spiked Concentration (mg/m3) Spike recovery (%) Final spike recovery P 2 PS (%) Ammonia 7664-41-7 0.667 0.507 1.11 86.7 ～ 100 91.2 ± 8.6 0.200 0.096 0.278 85.8 ～ 103 90.9 ± 13.0 Methylamine 74-89-5 1.67 ND1.72 100 ～ 106 103 ± 3.4 0.100 ND0.104 94.7 ～ 112 104 ± 10.0 Dimethylamine 1.67 ND1.75 100 ～ 110 105 ± 6.0 0.100 ND0.105 97.0 ～ 114 105 ± 9.6 Trimethylamine 1.67 0.777 2.39 92.7 ～ 103 96.8 ± 7.2 0.100 0.076 0.169 88.6 ～ 101 93.2 ± 10.4 ......

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