|
US$189.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email.
HJ 789-2016: Water quality. Determination of Acetonitrile. Direct injection /Gas chromatography
Status: Valid
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| HJ 789-2016 | English | 189 |
Add to Cart
|
3 days [Need to translate]
|
Water quality. Determination of Acetonitrile. Direct injection /Gas chromatography
| Valid |
HJ 789-2016
|
PDF similar to HJ 789-2016
Basic data | Standard ID | HJ 789-2016 (HJ789-2016) | | Description (Translated English) | Water quality. Determination of Acetonitrile. Direct injection /Gas chromatography | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Word Count Estimation | 8,838 | | Date of Issue | 2016-03-29 | | Date of Implementation | 2016-05-01 | | Quoted Standard | HJ/T 91; HJ/T 164 | | Regulation (derived from) | Ministry of Environmental Protection Announcement No | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 789-2016: Water quality. Determination of Acetonitrile. Direct injection /Gas 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.
Water quality.Determination of Acetonitrile.Direct injection/Gas chromatography
National Environmental Protection Standard of the People 's Republic of China
Determination of water quality of acetonitrile
Direct Injection/Gas Chromatography
Water quality-Determination of Acetonitrile
Direct injection/Gas chromatography
2016-03-29 released
2016-05-01 implementation
release
Ministry of Environmental Protection
Directory
Preface .ii
1 Scope of application
2 normative reference documents
3 Principle of the method
4 reagents and materials 1
5 instruments and equipment 2
6 Sample 2
7 Analysis steps
8 results are calculated and expressed
9 precision and accuracy
10 quality assurance and quality control 4
11 Waste treatment .5
12 Precautions
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 China on the Prevention and Control of Water Pollution,
Protection of human health, regulate the determination of acetonitrile in water, the development of this standard.
This standard specifies the direct injection/gas chromatography for the determination of acetonitrile in water.
This standard is the first release.
This standard is organized by the Ministry of Environmental Protection Science and Technology Standards Division.
The main drafting unit of this standard. Dalian Environmental Monitoring Center.
The standard verification unit. Liaoning Province Environmental Monitoring Experimental Center, Shenyang City Environmental Monitoring Center Station, Jinzhou City Environmental Monitoring
Central station, Tianjin Environmental Monitoring Center, Jiangsu Province Environmental Monitoring Center and Suzhou Environmental Monitoring Center Station.
The environmental protection department of this standard approved on March 29,.2016.
This standard has been implemented since May 1,.2016.
This standard is explained by the Ministry of Environmental Protection.
Water quality - Determination of acetone - Direct injection/gas chromatography
Warning. The acetonitrile used in the experiment is harmful to human health. The standard solution preparation process should be carried out in the fume hood.
Should be required to wear protective equipment, to avoid contact with skin and clothing.
1 Scope of application
This standard specifies the direct injection/gas chromatography for the determination of acetonitrile in water.
This standard is applicable to the determination of acetonitrile in surface water, groundwater, industrial waste water and domestic sewage.
When the injection volume was 1.0 μl, the detection limit of acetonitrile was 0.04 mg/L and the lower limit was 0.16 mg/L.
2 normative reference documents
The contents of this standard refer to the following documents or their terms. Those who do not specify the date of the reference file, the effective version of the appropriate
For this standard.
Technical specification for surface water and wastewater monitoring
Technical specification for groundwater environmental monitoring
3 Principle of the method
The filtered samples were injected directly into a gas chromatograph and separated by a column and tested with a nitrogen and phosphorus detector. To keep
Qualitative and external standard method.
4 reagents and materials
4.1 Experimental water. secondary distilled water or water prepared by pure water equipment.
Before use, subject to a blank test to confirm that there is no interference to the target compound in the retention time interval or target combination
The detection concentration is lower than the method detection limit.
4.2 acetonitrile (CH3CN). pure chromatography.
4.3 acetonitrile standard stock solution. ρ (CH3CN) ≈ 1 × 103 mg/L.
Prepared with acetonitrile (4.2) at room temperature at 20 ° C. Remove the appropriate amount of test water (4.1) in a 100 ml volumetric flask
(4.2) to about 100 mg (accuracy to 0.1 mg), and weigh again, according to
The difference between the two weighing weights determines the exact addition of acetonitrile. With the experimental water (4.1) constant volume to the mark, shake, calculate the standard
The exact concentration of the quasi-stock solution (accurate to 1 mg/L). Transfer to a brown reagent bottle equipped with a polytetrafluoroethylene screw cap at 4 ° C
The following cold storage, dark and sealed can be kept for 3 months. You can also purchase commercially available certified materials (in water as solvent).
4.4 acetonitrile standard use of liquid. ρ (CH3CN) = 10.0 mg/L.
(4.1) and a certain volume of acetonitrile standard stock solution (4.3) in a 100 ml volumetric flask,
Experimental water (4.1) constant volume to the mark, shake. Pro is now available.
4.5 high purity nitrogen. purity ≥ 99.999%.
4.6 Hydrogen. purity ≥99.95%.
4.7 Air. Dehumidified silica gel dehumidification and dehydrocarbon removal of hydrocarbons, or oil-free compressed air purified by 5 Å molecular sieve.
4.8 Water phase needle filter. Polyethersulfone or mixed cellulose ester, 13 mm × 0.45 μm.
5 instruments and equipment
Unless otherwise stated, the use of the national standard A-class glass gauge is used for the analysis.
5.1 Gas Chromatograph. with capillary column shunt/splitless inlet, equipped with nitrogen and phosphorus detector (NPD).
5.2 Column. quartz capillary column, 30 m x 0.32 mm, film thickness 1.0 μm (polyethylene glycol -20 M fixative), or
Other equivalent columns.
5.3 Reagent Bottle. 100 ml brown reagent bottle with polytetrafluoroethylene screw cap.
5.4 Sampling vials. 40 ml brown wide mouth sampling vial with PTFE cap screw cap.
5.5 Vials. 2 ml, equipped with polytetrafluoroethylene liner screw cap.
5.6 balance. one thousandth of a balance.
5.7 Volumetric flask. Class A, 100 ml.
5.8 General laboratory equipment and equipment commonly used.
6 samples
6.1 Collection of samples
Refer to the relevant provisions of HJ/T 91 and HJ/T 164. Use a 40 ml brown wide mouth with a Teflon screw cap
Sampling bottle (5.4) Samples are collected and the collected sample should be filled with sampling vials and sealed. Each batch of samples should be at least one full
The procedure is blank (with the same batch of experimental water instead of the sample).
6.2 Transport and storage of samples
After the collection of samples should be refrigerated below 4 ℃, dark, sealed and transported. If not timely analysis, should be at 4 ℃ to
Under the cold storage, dark and sealed preservation, storage period of not more than 6 d. There should be no organic interference in the sample storage area.
6.3 Preparation of the sample
The collected samples were filtered to a 2 ml vial (5.5) with an aqueous needle filter (4.8), to be tested.
7 Analysis steps
7.1 Chromatographic analysis of the reference conditions
Injection volume of 1.0 μl; inlet temperature of 220 ° C; splitless injection, splitless injection time of 0.75 min; column
The tank temperature was 50 ° C; the column flow rate was 5.0 ml/min; the detector temperature was 330 ° C, the hydrogen flow rate was 3.5 ml/min, the air flow
The amount of 80 ml/min.
7.2 Drawing of standard curves
Remove the appropriate amount of test water (4.1) in 5 100 ml brown volumetric flask, respectively, add 1.0 ml, 5.0 ml, 10.0
Ml, 20.0 ml, 50.0ml acetonitrile standard use of liquid (4.4), with the experimental water volume to the mark, shake. Formulated into acetonitrile quality
Concentration of 0.10 mg/L, 0.50 mg/L, 1.00 mg/L, 2.00 mg/L, 5.00 mg/L standard solution,
Degree of 10.0 mg/L acetonitrile standard using the liquid (4.4) combined into a standard series of 6 mass concentrations. From low to high concentrations
Remove the 1.00 μl into the gas chromatograph and proceed to the chromatographic analysis reference conditions (7.1). To standard series of thick
(Mg/L) is the abscissa, and the standard curve is established with the corresponding peak area (or peak height) of the chromatogram.
7.3 Standard reference chromatogram
Under the reference conditions (7.1) of the chromatographic analysis given in this standard, the acetonitrile standard gas chromatogram is shown in Figure 1.
Figure 1 acetonitrile standard chromatogram
7.4 Determination of sample
The sample was measured according to the same chromatographic analysis reference conditions (7.1) and (7.2) as the standard curve.
7.5 blank test
The same chromatographic analysis reference conditions (7.1) and (7.4) were used in the same batch of experimental water instead of the sample,
Perform a blank test.
Calculation and representation of results
8.1 Qualitative analysis of acetonitrile
The target is qualitatively based on the retention time of the target in the sample and the target in the standard series. Before the sample analysis,
Create retention time window t ± 3s. T for the initial calibration, the concentration level of acetonitrile retention time average, s for the initial calibration of the
Standard deviation of acetonitrile retention time at the concentration level. When the sample is analyzed, the target should peak within the retention time window.
Quantitative analysis of acetonitrile
8.2.1 Result calculation
From the standard curve, the concentration of acetonitrile was 1ρ, the concentration of acetonitrile in the water sample was calculated according to the formula (1)
F × = 1ρρ (1)
Where. ρ - the mass concentration of acetonitrile in the sample, mg/L;
1ρ - the acetonitrile concentration obtained from the standard curve, mg/L;
F - sample dilution factor.
8.2.2 result representation
When the determination result is less than 1 mg/L, two decimal places are retained; when the result is greater than or equal to 1 mg/L,
Bit effective number.
9 precision and accuracy
9.1 precision
Six laboratories with a concentration of 0.10 mg/L acetonitrile, 5.00 mg/L, 9.00 mg/L of the uniform blank spiked samples were measured
The relative standard deviations in the laboratory were 4.3% ~ 9.3%, 1.9% ~ 6.3%, 0.8% ~ 5.0%, respectively.
The quasi-deviations were 2.8%, 2.3% and 0.5%, respectively. The reproducibility limits were 0.02 mg/L, 0.52 mg/L, 0.67 mg/L, respectively
The limits were. 0.02 mg/L, 0.58 mg/L, 0.62 mg/L, respectively.
Six laboratories were tested for surface water samples with a standard concentration of 0.10 mg/L and 5.00 mg/L.
The quasi-deviations were 4.6% ~ 6.9%, 1.9% ~ 3.2%, respectively. The relative standard deviations were 11% and 6.0%, respectively.
The limits were 0.02 mg/L, 0.36 mg/L, respectively. The reproducibility limits were 0.03 mg/L and 0.90 mg/L, respectively.
The concentration of the two laboratories was 0.12 mg/L ~ 0.15 mg/L, 1.42 mg/L ~ 1.63 mg/L, 7.13 mg/L ~ 7.52 mg/L
Of the actual sample of waste water were measured. the relative standard deviation of the laboratory were 7.0% ~ 11%, 3.4% ~ 7.7%, 1.9% ~
2.9%.
9.2 Accuracy
Six laboratories with a concentration of 0.10 mg/L acetonitrile, 5.00 mg/L, 9.00 mg/L of the uniform blank spiked samples were measured
The recoveries were 94.6% ~ 102%, 94.2% ~ 100%, 98.2% ~ 99.6%, respectively. The final recoveries were
Not 96.9% ± 5.4%, 98.1% ± 4.6%, 98.7% ± 1.2%.
Six laboratories were tested for surface water samples with a standard concentration of 0.10 mg/L and 5.00 mg/L.
88.0% ~ 114%, 91.0% ~ 107%, and the final recoveries were 101% ± 22% and 99.7% ± 12.0%, respectively.
Six laboratories for the standard concentration of 0.20 mg/L, 3.00 mg/L, 8.00 mg/L of the actual sample of wastewater determination.
The recoveries were 96.5% ~ 108%, 92.7% ~ 103%, 96.0% ~ 103%, respectively. The final recoveries were
102% ± 8.8%, 98.2% ± 8.8%, 99.5% ± 6.2%.
10 quality assurance and quality control
10.1 Calibration
The standard curve should be drawn for each batch, and the correlation coefficient should be ≥ 0.995. Otherwise, you should find the reason to redraw the standard curve.
For each 20 samples or per batch (less than 20 samples) a standard curve should be measured in the middle of the standard solution, the test
The relative error between the result and the standard curve should be ≤ ± 15%. Otherwise, the standard curve must be redrawn.
10.2 blank test
Every 20 samples or per batch (less than 20 samples) should analyze at least one lab blank and one full program blank.
The determination of acetonitrile in the blank should be lower than the method detection limit.
10.3 spiked samples
Every 20 samples or each batch (less than 20 samples) should be analyzed at least one blank plus standard and one sample plus standard,
The recoveries should be in the range of 85% to 115%.
10.4 parallel samples
Every 10 samples or each batch (less than 10 samples) should be analyzed for at least one parallel sample, parallel to the sample
The deviation should be ≤ 15%.
11 Waste treatment
The acetonitrile waste generated in the experiment should be collected and kept collectively and commissioned by qualified units for processing.
12 Precautions
12.1 Glassware containing trace amounts of chromium will affect the determination of chromium and acetonitrile. Should choose chrome-free sampling and
Analytical containers.
12.2 Since the water in the sample and standard series affects the stability of the column to a certain extent, if the baseline is unstable or
Other interference, the need to heat aging column.
12.3 to avoid nitrogen and phosphorus detector bead deliquescence, should be a week to start running once, so that nitrogen and phosphorus detector temperature.
Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of HJ 789-2016_English be delivered?Answer: Upon your order, we will start to translate HJ 789-2016_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 789-2016_English with my colleagues?Answer: Yes. The purchased PDF of HJ 789-2016_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.
|