US$279.00 · In stock Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. HJ 688-2019: Stationary source emission--Determination of hydrogen fluoride--Ion chromatography Status: Valid HJ 688: Evolution and historical versions
Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
HJ 688-2019 | English | 279 |
Add to Cart
|
3 days [Need to translate]
|
Stationary source emission--Determination of hydrogen fluoride--Ion chromatography
| Valid |
HJ 688-2019
|
HJ 688-2013 | English | 439 |
Add to Cart
|
3 days [Need to translate]
|
Stationary source emission. Determination of hydrogen fluoride. Ion chromatography
| Obsolete |
HJ 688-2013
|
PDF similar to HJ 688-2019
Basic data Standard ID | HJ 688-2019 (HJ688-2019) | Description (Translated English) | Stationary source emission--Determination of hydrogen fluoride--Ion chromatography | Sector / Industry | Environmental Protection Industry Standard | Classification of Chinese Standard | Z15 | Classification of International Standard | 13.040.40 | Word Count Estimation | 12,138 | Date of Issue | 2019 | Date of Implementation | 2020-06-30 | Issuing agency(ies) | Ministry of Ecology and Environment |
HJ 688-2019: Stationary source emission--Determination of hydrogen fluoride--Ion chromatography ---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.
Stationary source emission--Determination of hydrogen fluoride--Ion chromatography
National Environmental Protection Standard of the People's Republic of China
Replaces HJ 688-2013
Determination of hydrogen fluoride in exhaust gas from stationary pollution sources
Ion chromatography
Stationary source emission-Determination of hydrogen fluoride
-Ion chromatography
2019-12-31 released
2020-06-30 implementation
Released by the Ministry of Ecology and Environment
i table of contents
Foreword ... ii
1 Scope ... 1
2 Normative references ... 1
3 Terms and definitions ... 1
4 Methodology ... 1
5 Interference and cancellation ... 2
6 Reagents and materials ... 2
7 Instruments and equipment ... 2
8 Sample ... 3
9 Analysis steps ... 5
10 Calculation and Representation of Results ... 6
11 Precision and accuracy ... 7
12 Quality Assurance and Quality Control ... 7
13 Waste disposal ... 8
14 Notes ... 8
Foreword
In order to implement the "Environmental Protection Law of the People's Republic of China"
Environment, protect human health, standardize the determination method of hydrogen fluoride in exhaust gas from fixed pollution sources, and formulate this standard.
This standard specifies ion chromatography for the determination of hydrogen fluoride in exhaust gas from stationary sources.
This standard is for the determination of hydrogen fluoride in exhaust gas from stationary sources by ion chromatography (Interim) (HJ 688-2013)
Revision.
This standard was first published in.2013. The original drafting unit was Dongying City Environmental Monitoring Station. This is the first revision.
The main contents of the amendment are as follows.
-The scope of application was modified, and the method detection limit and determination lower limit were changed;
-Revised normative references;
-Improved sample collection, processing and storage methods;
-Refine the chromatographic reference conditions and increase the ion chromatogram of the target component;
-Revised the result expression formula and result expression requirements;
-Improved the terms of quality assurance and quality control and precautions;
-Added warnings, terms and definitions, interference and elimination, precision and accuracy clauses.
From the date of implementation of this standard, the original standard "Determination of hydrogen fluoride in stationary pollution sources by ion chromatography (interim)"
(HJ 688-2013) Repealed.
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. Shandong Dongying Ecological Environment Monitoring Center, China University of Petroleum (East China).
Verification units of this standard. Shandong Ecological Environment Monitoring Center, Shandong Tai'an Ecological Environment Monitoring Center, Shandong Province
Bo Ecological Environment Monitoring Center, Shandong Weifang Ecological Environment Monitoring Center, China University of Petroleum (East China) Dongying Zhongshi University
Petroleum and Petrochemical Testing and Evaluation Center and Qingdao Institute of Bioenergy and Process, Chinese Academy of Sciences.
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.
1 Determination of hydrogen fluoride in exhaust gas from stationary sources Ion chromatography
Warning. Hydrogen fluoride is harmful to the human body. Take precautions when taking samples to avoid inhalation or contact with skin and eyes. Make use of
The sodium hydroxide and potassium hydroxide used are strongly corrosive. Reagent preparation and sample preparation should avoid contact with skin and
Clothing.
1 Scope
This standard specifies ion chromatography for the determination of hydrogen fluoride in exhaust gas from stationary sources.
This standard applies to the determination of hydrogen fluoride in exhaust gas from stationary pollution sources.
When the sampling volume is 20 L (standard state) and the constant volume is 100 ml, the method detection limit is 0.08 mg/m3.
The lower limit of determination is 0.32 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.
GB/T 16157 Determination of particulate matter and sampling of gaseous pollutants in exhaust from stationary pollution sources
HJ/T 47 Technical Specifications of Flue Gas Sampler
HJ/T 48 Soot Sampler Technical Specifications
HJ/T 397 Fixed source exhaust gas monitoring technical specifications
3 terms and definitions
The following terms and definitions apply to this standard.
3.1
Hydrogen fluoride
The hydrogen fluoride measured in this standard refers to inorganic fluorides such as hydrogen fluoride and silicon tetrafluoride (as fluorine
Hydrogen meter).
4 Method principle
The heated sampling tube is used to collect the exhaust gas sample, and the particulate matter, gaseous hydrogen fluoride and gasified hydrogen fluoride are removed by a filtering membrane.
The droplets are absorbed by the alkaline absorbent to generate fluoride ions. The sample is injected into the ion chromatograph for separation and detection.
Quantitatively, peak area or peak height.
25 Interference and cancellation
5.1 Particulate fluoride interferes with the measurement. Use a filter to remove it during sampling.
5.2 Acetate ions interfere with the determination of fluoride. You can adjust the eluent concentration and flow rate, and replace the high-efficiency special chromatography.
Column and other methods to eliminate and reduce its interference.
6 Reagents and materials
Unless otherwise stated, all analytical reagents in accordance with national standards are used in the analysis. The resistivity of experimental water is ≥
18 MΩ · cm deionized water.
6.1 Potassium hydroxide (KOH). excellent grade pure.
6.2 Sodium hydroxide (NaOH). excellent grade pure.
6.3 Sodium carbonate (Na2CO3). Excellent grade. It should be dried at 105 ° C ± 5 ° C and constant weight before use and stored in a desiccator.
6.4 Sodium bicarbonate (NaHCO3). Excellent grade. It should be placed in a desiccator for 24 h before use.
6.5 Sodium fluoride (NaF). Excellent grade. It should be dried at 105 ° C ± 5 ° C before use and kept in a desiccator.
6.6 Aqueous solution absorption solution. c (KOH) = 30 mmol/L or c (NaOH) = 30 mmol/L.
Weigh 1.68 g of potassium hydroxide (6.1) or 1.20 g of sodium hydroxide (6.2), dissolve in an appropriate amount of water and transfer to 1000 ml
In a volumetric flask, dilute to volume with water, mix well, and transfer to a polyethylene bottle. Provisional use.
6.7 Eluent. Prepare according to the instrument model and the operating conditions of the column manual. The eluent conditions given below are provided
reference.
6.7.1 Carbonate eluent. c (Na2CO3) = 3.2 mmol/L, c (NaHCO3) = 1.0 mmol/L.
Accurately weigh 0.6784 g of sodium carbonate (6.3) and 0.1680 g of sodium bicarbonate (6.4), respectively, and dissolve them in an appropriate amount of water.
Transfer the volume to a.2000 ml volumetric flask, dilute to volume with water, and mix.
6.7.2 Hydroxide eluent. Generated by the eluent automatic electrolytic generator online.
Note. The eluent should be degassed before use to prevent air bubbles from entering the ion chromatography system.
6.8 Fluoride stock solution. ρ (F-) = 500 mg/L.
Accurately weigh 1.1053 g of sodium fluoride (6.5), dissolve it in an appropriate amount of water, transfer it to a 1000 ml volumetric flask, and dilute with water
Make up to volume, mix well, transfer to a polyethylene bottle, and refrigerate at 4 ° C for a month.
They can also be formulated using certified standard solutions.
6.9 Fluoride standard solution. ρ (F-) = 50 mg/L.
Pipette 10.00 ml of sodium fluoride stock solution (6.8), transfer to a 100 ml volumetric flask, dilute to volume with water, mix well,
Store at room temperature for 14 days.
6.10 Filter membrane. Teflon material, the retention efficiency for particles larger than 0.3 μm is not less than 99.9%.
7 instruments and equipment
7.1 Constant temperature heating sampling tube
A filter membrane (6.10) is installed at the end of the constant temperature heating sampling tube. The heating temperature is 120 ° C ± 5 ° C and the temperature control accuracy is 1 ° C. Sampling tube
3 is made of polytetrafluoroethylene or titanium alloy, and the inner surface is smooth.
7.2 Flue gas sampler
The flue gas sampler shall meet the technical requirements of HJ/T 47.
7.3 Smoke Sampler
The dust sampler should meet the technical requirements of HJ/T 48 and be equipped with a flow controllable shunt device.
7.4 Absorption bottle. 75 ml bubble absorption bottle made of PTFE, polyethylene or polypropylene.
7.5 Connection tube. PTFE hose or silicone rubber tube lined with PTFE film should be as short as possible.
7.6 Membrane clip. PTFE material, the size matches the filter membrane (6.10).
7.7 Cooling device. Use ice-water bath or other device whose temperature does not exceed 5 ℃.
7.8 Ion chromatograph. An analysis system consisting of an ion chromatograph host, operating software, and required accessories. Equipped with anion
Off-column (polydivinylbenzene/ethylvinylbenzene/polyvinyl alcohol matrix, with alkanol quaternary ammonium or alkyl quaternary ammonium functional group, hydrophilic,
High-capacity chromatography columns), anion guard columns, and conductivity detectors are suitable for the detection of fluoride ions.
7.9 Disposable water-based microfiltration membrane syringe filter. 0.45 µm pore size.
7.10 Syringe. 10 ml.
7.11 Instruments and equipment commonly used in general laboratories.
8 samples
8.1 Sample collection
8.1.1 Exhaust gas samples from stationary sources
The location and sampling of exhaust gas from fixed pollution sources shall comply with the relevant regulations in GB/T 16157 and HJ/T 397. For sampling devices, see
figure 1. During the sampling process, the temperature of the sampling tube and filter should be maintained at ≥120 ° C to avoid condensation of water vapor before the absorption bottle.
Figure 1 Schematic diagram of sampling device for hydrogen fluoride in exhaust gas from stationary pollution sources
Fig. 2 Schematic diagram of sampling device for hydrogen fluoride in exhaust gas from stationary pollution source (when it contains droplets)
After the sampling tube (7.1), two 75 ml bubble absorption bottles (7.4) each containing 50 ml of absorption liquid (6.6) are connected in series, and
The flue gas sampler (7.2) is connected. According to the gaseous pollutant collection method, the flow rate is 0.5 L/min ~ 1.0 L/min within 1 hour
3 to 4 samples are taken at equal time intervals or samples are collected continuously for 1 hour. It can also be based on the actual concentration of the sample in the exhaust gas.
Degree, appropriately extend or shorten the sampling time.
Note. When the moisture content in the exhaust gas from the fixed pollution source is relatively large, and the moisture absorption of hydrogen fluoride exists in the form of mist droplets, the layout and sampling should comply with GB/T
The provisions of 16157 and HJ/T 397 on the collection methods of particulate matter, the sampling device is shown in Figure 2. Two tubes in series after the sampling tube (7.1)
75 ml bubble absorption bottles (7.4) each containing 50 ml of absorption solution (6.6), connected to the smoke sampler (7.3), collected according to the particulate matter
Set method to collect gas samples. Through the diverter valve, control the sampling flow rate of hydrogen fluoride gas from 0.5 L/min to 1.0 L/min, at 1
Sampling 3 to 4 samples at equal intervals within one hour or continuous 1 hour sampling.
8.1.2 Blanks throughout the program
Each batch of samples should bring at least a set of full-process blank samples, and bring the absorption bottle filled with the absorption liquid to the sampling site.
It is not connected to the sampler and will be taken back to the laboratory for testing after the sampling is completed.
8.2 Sample transport and storage
After the sample was collected, the absorption bottle was sealed with a connecting tube (7.5), and stored at room temperature. The analysis and measurement were completed within 24 hours. If not
During analysis, the sample should be transferred to a polyethylene bottle, which can be stored at room temperature for 14 days.
8.3 Preparation of test specimens
8.3.1 Exhaust gas samples from stationary sources
Transfer the sample solution (8.1.1 and 8.1.2) from the two absorption bottles into two 100 ml stoppered colorimetric tubes.
Measure the water to wash the absorption bottle and the inner wall of the connecting tube.
58.3.2 Laboratory blank sample
In the laboratory, take the same batch of absorbent bottles with the same volume of absorbent solution and prepare the laboratory empty according to the same steps in 8.3.1.
White sample.
9 Analysis steps
9.1 Chromatographic Reference Conditions
Optimize the measurement conditions or parameters according to the instrument model and configuration, and optimize the eluent concentration
degree.
Reference condition 1. eluent is 30 mmol/L potassium hydroxide solution, flow rate is 1.20 ml/min, injection volume is 25 µl,
The column temperature was 30 ° C and the suppressor current was 90 mA.
Reference condition 2. The eluent is a mixed solution of 3.2 mmol/L sodium carbonate and 1.0 mmol/L sodium bicarbonate, and the flow rate is
0.40 ml/min, injection volume is 20 µl, and column temperature is 25 ° C.
9.2 Standard curve establishment
Remove 0 ml, 0.10 ml, 0.20 ml, 0.50 ml, 1.00 ml, 2.00 ml, 5.00 ml of fluoride standard
Place the solution (6.9) in a set of 50 ml volumetric flasks, make up to volume with water, and shake well. Fluoride ion concentration in the standard series
(Calculated as F-) 0.00 mg/L, 0.10 mg/L, 0.20 mg/L, 0.50 mg/L, 1.00 mg/L, 2.00 mg/L and
5.00 mg/L. The appropriate standard series concentration range can be determined based on the concentration of the sample being measured. Standards of different concentrations
The solution is injected into the ion chromatograph, and the response value and retention time of the instrument are measured. With fluoride ion concentration (calculated as F-, mg/L) as the horizontal
Coordinate, peak area or peak height is the ordinate, and a standard curve is established. The fluoride ion chromatogram in the hydroxide eluent system is shown in Figure 3.
The fluoride ion chromatogram in the carbonate eluent system is shown in Figure 4.
1-fluoride ion; 2-chloride ion; 3-sulfate ion; 4-bromide ion; 5-nitrate ion.
Figure 3 Chromatogram of fluoride standard ion (hydroxide eluent system)
61-fluoride ion; 2-chloride ion; 3-bromide ion; 4-nitrate ion; 5-sulfate ion.
Figure 4 Chromatogram of fluoride standard ion (carbonate eluent system)
9.3 Sample measurement
The prepared samples (8.3.1 and 8.3.2) are filtered with a disposable water-based microporous membrane syringe filter (7.9) and then injected.
The injector (7.10) is injected into the ion chromatograph, and the same chromatographic reference conditions (9.1) are used to establish the standard curve as the sample.
Determination. When the F-content in the sample exceeds the concentration range of the standard curve, it shall be determined after dilution with water.
10 Calculation and representation of results
10.1 Calculation of results
The concentration of hydrogen fluoride in the exhaust gas from the stationary pollution source is calculated according to formula (1).
0.19
0.20100) (2211
) (
nd
HF V
DD (1)
Where. ρ (HF)-the concentration of HF in the exhaust gas from a fixed pollution source, mg/m3;
ρ1--F after dilution of the first colorimetric tube sample detected from the standard curve
-Concentration, mg/L;
ρ2--F after dilution of the second colorimetric tube sample detected from the standard curve
-Concentration, mg/L;
Vnd--Sampling volume of dry flue gas under standard conditions (273.15K, 1013.25hPa), L;
Molar mass of 20.0--HF, g/mol;
Molar mass of 19.0--F-, g/mol;
100--constant volume, ml;
D1--the dilution factor of the first colorimetric tube sample;
D2--The dilution factor of the second colorimetric tube sample.
Note. If ρ2 is lower than the detection limit of the method, ρ2 is counted as zero.
10.2 Results representation
7 The number of reserved digits after the decimal point of the measurement result is consistent with the detection limit, and a maximum of three significant digits are retained.
11 Precision and accuracy
11.1 Precision
Six verification laboratories added blank spiked concentrations of 0.20 mg/L, 2.00 mg/L, and 8.00 mg/L, respectively.
Six parallel determinations of the standard sample after the sampling process.
Relative standard deviations in the laboratory are. 1.1% to 11%, 0.8% to 6.0%, 0.3% to 2.5%;
The relative standard deviations between laboratories were. 7.1%, 2.3%, and 1.8%;
Repeatability limits are. 0.11 mg/m3, 0.54 mg/m3, and 0.92 mg/m3;
Reproducibility limits were. 0.15 mg/m3, 0.65 mg/m3, and 1.4 mg/m3.
Six verification laboratories simulated actual samples of 0.50 mg/m3 and 10.0 mg/m3 hydrogen fluoride standard gases, respectively.
Perform 6 parallel determinations.
The relative standard deviations in the laboratory are. 2.3% to 7.6% and 1.9% to 4.0%;
The relative standard deviations between the laboratories are 4.2% and 2.7%;
Repeatability limits are. 0.10 mg/m3 and 0.82 mg/m3;
Reproducibility limits were 0.12 mg/m3 and 1.1 mg/m3, respectively.
11.2 Accuracy
Six verification laboratories have performed a unified standard sample (standard value of 1.53 mg/L ± 0.06) containing fluoride (calculated as F-)
mg/L) 6 parallel determinations.
The relative errors are. -3.3% to 1.5%;
The final relative error is -1.0% ± 3.6%.
Six verification laboratories simulated the sampling process of solutions containing 10.0 μg, 50.0 μg, and.200 μg of fluoride ions
After recovery measurement.
Spike recovery rates were 88.8% ~ 111%, 92.4% ~ 112%, 96.3% ~ 106%;
The final recoveries were spiked at 101% ± 17.5%, 103% ± 14.4%, and 101% ± 6.6%.
12 Quality Assurance and Quality Control
12.1 Blank test
At least one full program blank and one experiment per 20 samples or each batch (less than 20 samples/batch)
Room is blank. The blank measurement value should be lower than the detection limit of the method, otherwise the cause should be found or the sample should be collected again.
12.2 Calibration curve
When making the standard curve, there should be at least six concentration points including the zero concentration point, and the linear correlation coefficient of the standard curve should be
Should be ≥0.995. For every 20 samples or each batch (less than 20 samples/batch), the middle concentration point of the standard curve should be used.
Check the relative error should be within ± 10%. Otherwise, find the cause or re-establish the standard curve.
812.3 Penetration
The content of hydrogen fluoride in the second absorption bottle should be less than 10% of the total hydrogen fluoride sample, otherwise the sample should be collected again. press
Calculate the transmittance of the second absorption bottle according to formula (2).
100%
22
DD
K
(2)
In the formula. K--penetration of the second absorption bottle;
ρ1--F after dilution of the first colorimetric tube sample detected from the standard curve
-Concentration, mg/L;
ρ2--F after dilution of the second colorimetric tube sample detected from the standard curve
-Concentration, mg/L;
100--constant volume, ml; D1--the dilution factor of the first colorimetric tube sample;
D2--The dilution factor of the second colorimetric tube sample.
13 Waste treatment
The waste liquid and waste generated in the experiment should be collected separately and properly stored, safely processed as required or entrusted to a qualified unit
For processing.
14 Notes
14.1 Titanium alloy is chemically inert, has a smooth surface, and is resistant to corrosion. It can be used at temperatures between 450 ° C and 550 ° C. Teflon
The use temperature of ethylene must not be higher than 250 ° C, otherwise it will decompose and release fluoride. New PTFE devices may release fluorine
The compound gas needs to be heated in advance at the sampling temperature.
14.2 The connecting tube between the filter holder and the absorption bottle should be as short as possible, and the airtightness of the system should be checked.
14.3 The connection tube between the filter holder and the absorption bottle is kept in a gentle downward manner to prevent water vapor in the sample gas from cooling in the connection tube.
After coagulation, it was returned to the filter holder.
14.4 After the analysis of each sample, the eluent should be used to clean the instrument pipeline.
14.5 This method has high sensitivity. The absorption bottle, connection tube and utensils should be washed carefully. Prevent the residual fluorination of utensils during operation
Interference from chemicals, tap water and air.
Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of HJ 688-2019_English be delivered?Answer: Upon your order, we will start to translate HJ 688-2019_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. The lengthier the document the longer the lead time. Question 2: Can I share the purchased PDF of HJ 688-2019_English with my colleagues?Answer: Yes. The purchased PDF of HJ 688-2019_English will be deemed to be sold to your employer/organization who actually pays for it, including your colleagues and your employer's intranet. Question 3: Does the price include tax/VAT?Answer: Yes. Our tax invoice, downloaded/delivered in 9 seconds, includes all tax/VAT and complies with 100+ countries' tax regulations (tax exempted in 100+ countries) -- See Avoidance of Double Taxation Agreements (DTAs): List of DTAs signed between Singapore and 100+ countriesQuestion 4: Do you accept my currency other than USD?Answer: Yes. If you need your currency to be printed on the invoice, please write an email to [email protected]. In 2 working-hours, we will create a special link for you to pay in any currencies. Otherwise, follow the normal steps: Add to Cart -- Checkout -- Select your currency to pay. Question 5: Should I purchase the latest version HJ 688-2019?Answer: Yes. Unless special scenarios such as technical constraints or academic study, you should always prioritize to purchase the latest version HJ 688-2019 even if the enforcement date is in future. Complying with the latest version means that, by default, it also complies with all the earlier versions, technically.
|