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HJ 756-2015: Water quality. Determination of butyl xanthate. UV spectrophotometric method
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Water quality. Determination of butyl xanthate. UV spectrophotometric method
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HJ 756-2015
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Standard similar to HJ 756-2015 HJ 511 HJ 945.3 HJ 943 Basic data | Standard ID | HJ 756-2015 (HJ756-2015) | | Description (Translated English) | Water quality. Determination of butyl xanthate. UV spectrophotometric method | | Sector / Industry | Environmental Protection Industry Standard | | Word Count Estimation | 9,995 | | Date of Issue | 2015-10-22 | | Date of Implementation | 2015-12-01 | | Quoted Standard | HJ/T 91; HJ/T 164 | | Regulation (derived from) | Ministry of Environment Announcement 2015 No.62 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This standard specifies the Determination of UV-butyl xanthan spectrophotometry. This standard applies to surface water, groundwater, sewage and industrial waste water was measured in the butyl xanthate. The standard detection limit of 0.004mg/L, detection limit of 0.016mg/L. | HJ 756-2015: Water quality. Determination of butyl xanthate. UV spectrophotometric method---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 butyl xanthate.UV spectrophotometric method
National Environmental Protection Standard of the People's Republic
Determination of water quality butyl xanthogen
UV spectrophotometry
Water quality-Determination of butyl xanthate-UV spectrophotometric
Method
Published on.2015-10-22
2015-12-01 Implementation
Ministry of Environmental Protection released
i directory
Foreword.ii
1 Scope.1
2 Normative references.1
3 Terms and Definitions 1
4 principle of the method.1
5 interference and elimination 1
6 Reagents and materials 1
7 Instruments and equipment 2
8 sample 2
9 Analysis steps. 2
10 Results calculation and representation.3
11 Precision and accuracy.3
12 Quality Assurance and Quality Control..3
13 Waste treatment 4
Foreword
To protect the environment and protect the human body 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 Water Pollution Prevention and Control
This standard is established for the determination of healthy, standardized butyl xanthogen in water.
This standard specifies the UV spectrophotometric method for the determination of butyl xanthogen 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. Shanghai Environmental Monitoring Center.
This standard is verified by. Nanjing Environmental Monitoring Center Station, Suzhou Environmental Monitoring Center Station, Ningbo Environmental Monitoring Station, Shanghai
Pudong New Area Environmental Monitoring Station, Shanghai Putuo District Environmental Monitoring Station, Shanghai Textile Energy Conservation and Environmental Protection Center.
This standard was approved by the Ministry of Environmental Protection on October 22,.2015.
This standard has been implemented since December 1,.2015.
This standard is explained by the Ministry of Environmental Protection.
1 Water quality butyl xanthic acid determination by ultraviolet spectrophotometry
1 Scope of application
This standard specifies the UV spectrophotometric method for the determination of butyl xanthogen in water.
This standard applies to the determination of butyl xanthogen in surface water, groundwater, domestic sewage and industrial wastewater.
The detection limit of this method is 0.004 mg/L, and the lower limit of determination is 0.016 mg/L.
2 Normative references
The contents of this standard refer to the following documents or their terms. For undated references, the valid version applies to this
standard.
HJ/T 91 Surface Water and Wastewater Monitoring Technical Specifications
HJ/T 164 Technical Specifications for Groundwater Environmental Monitoring
3 Terms and definitions
The following terms and definitions apply to this standard.
Butyl xanthate
Refers to the general name of the hydrocarbon-based xanthogenate in the sample measured under the conditions specified in this standard, based on butyl xanthogen.
4 Principle of the method
Butyl xanthogen is a hydrolysis product of xanthogenate. Butyl xanthate has a maximum absorption peak in the ultraviolet wavelength range, at pH< 2
The xanthogen is completely decomposed and the absorption peak disappears. Determination of acid by ultraviolet spectrophotometry at 301 nm
After the absorbance, the concentration of butyl xanthate was calculated from the difference in absorbance.
5 interference and elimination
The suspended insoluble matter in the water sample will cause interference, and the water sample to be tested is filtered through a 0.45 μm filter to remove the interference.
Nitrate has a positive interference at the absorption peak at 301 nm, but it can be offset during the experiment before and after the acid decomposition.
Influence measurement.
When the interference of the chromaticity of the sample cannot be removed, other method standards should be used.
6 reagents and materials
Analytically pure reagents in accordance with national standards were used for analysis, and the experimental water was newly prepared deionized water or steamed unless otherwise stated.
Distilled water.
6.1 Hydrochloric acid. ρ (HCl) = 1.19 g/ml.
6.2 Hydrochloric acid solution. 1 1.
6.3 Hydrochloric acid solution. c (HCl) = 0.01 mol/L.
Take 0.4 ml of hydrochloric acid (6.1) and dilute to 500 ml with water.
6.4 Sodium hydroxide solution. c (NaOH) = 0.01 mol/L.
Weigh 0.2 g of sodium hydroxide in a small amount of water and dilute to 500 ml.
26.5 Saturated sodium bicarbonate solution.
Weigh more than 9.6 g (at 20 ° C) sodium bicarbonate dissolved in 100 ml of water, should ensure that the bottom of the reagent bottle has sodium bicarbonate crystal precipitation.
6.6 butyl xanthogen standard stock solution. ρ (C4H9OCSSH) = 100 μɡ/ml.
Accurately weigh 0.0330 g (accurate to 0.1 mg) potassium butyl xanthate (C4H9OCSSK, content >95%) in a small amount of water,
Transfer to a 250 ml brown volumetric flask and bring to volume. It can be stored in a refrigerator at 4 ° C for one week.
Note 1. Butyl xanthate is easily decomposed by moisture, and the standard substance should be placed in a dark place and sealed.
6.7 Standard use solution of butyl xanthic acid. ρ (C4H9OCSSH) = 4.00 μɡ/ml.
Pipette 10.00 ml of butyl xanthogen standard stock solution (6.6) into a 250 ml brown volumetric flask and dilute to volume with water.
Available at the time of use.
6.8 Wash the solution.
Add 400 ml water, 100 ml 95% ethanol, 50 ml hydrochloric acid (6.1) to a 1000 ml container, mix and store in a reagent bottle.
Save.
Note 2. All glassware used should be cleaned with a cleaning solution and laboratory water.
7 Instruments and equipment
Unless otherwise stated, the analysis used a Class A glass gauge in accordance with national standards.
7.1 UV-Vis spectrophotometer with 30 mm quartz cuvette.
7.2 Filter, 0.45 μm.
7.3 Brown volumetric flask, 250 ml.
7.4 with a colorimetric tube, 25 ml.
7.5 Common instruments in general laboratories.
8 samples
8.1 Sample collection and preservation
The sample was collected in a brown glass bottle, and the pH of the water sample was adjusted with hydrochloric acid solution (6.3) or sodium hydroxide solution (6.4) immediately after collection.
Neutral, refrigerated at around 4 °C, complete sample analysis within 3 days.
8.2 Preparation of samples
The collected sample to be tested is turbid or contains insoluble substances, and it needs to be filtered with a 0.45 μm filter to remove the interference of insoluble substances.
9 Analysis steps
9.1 Drawing of the calibration curve
9.1.1 Add 0, 0.10, 0.50, 2.00, 7.00, 15.0 ml butyl xanthogen to a set of 6 colorimetric tubes (7.4).
The acid standard solution (6.7) is used, and the volume is adjusted to the scale with water, and the concentrations are 0, 0.016, 0.080, 0.320, 1.12, 2.40 mg/L, respectively.
Add 0.50 ml of water and shake well. The absorbance (A1) was measured at a wavelength of 301 nm using a 30 mm quartz cuvette with water as a reference.
9.1.2 Take another set of the same standard series tube (9.1.1), add 1 1 hydrochloric acid (6.2) 0.10 ml, adjust the pH to < 2, and let stand for 5 min.
Above, add 0.40 ml of saturated sodium bicarbonate solution (6.5), gently shake and deflate after capping, and let stand for 10 min. If it has a color
There are still bubbles in the tube, shake it again and deflate again. When the bubble is completely exhausted, take the water as a reference and measure the absorbance at 301 nm.
(A2). The absorbance [A= A1-(A2-A0)] is plotted on the ordinate, and the corresponding butyl xanthogen content (μg) is plotted on the abscissa.
Quasi-curve.
39.2 Determination
9.2.1 Take 1 sample of the appropriate amount in a plug colorimetric tube (7.4), dilute to the mark, add 0.50 ml of water, and shake. With 30 mm
The quartz cuvette was measured for its absorbance (A1) at a wavelength of 301 nm using water as a reference.
9.2.2 Take another sample of the same volume as (9.2.1) and carry out the acidification decomposition treatment of butylxanthate, the same procedure as in (9.1.2).
The absorbance is (A2).
9.3 Blank test
The blank test was carried out by replacing the sample with water, and the procedure was the same as (9.1), and the measured absorbance was A0.
10 Calculation and representation of results
10.1 Calculation of results
The value of absorbance A1-(A2-A0) is substituted into the calibration curve to calculate the content of butylxanthogen in the water sample to be tested.
mLmgC )/(
Where. C - butyl xanthogen concentration, mg/L;
m -- the content of butyl xanthogen in the sample, μg;
V -- the volume of the sample taken after pretreatment, ml.
10.2 Results are expressed
When the measurement result is less than 0.1 mg/L, the three decimal places are retained; when the measurement result is greater than or equal to 0.1 mg/L, the three positions are retained.
effective number.
11 Precision and accuracy
11.1 Precision
Six laboratories performed uniform samples containing butyl xanthogen concentrations of 0.048 mg/L, 0.800 mg/L, and 1.92 mg/L, respectively.
For the determination, the relative standard deviations in the laboratory were. 4.0~9.1%, 0.2~3.6%, 0.1~5.0%; the relative standard deviation between laboratories
They were. 4.6%, 1.9%, 3.6%; the repeatability limits were. 0.008 mg/L, 0.05 mg/L, 0.11 mg/L; the reproducibility limit was. 0.01
Mg/L, 0.06 mg/L, 0.21 mg/L.
11.2 Accuracy
6 laboratories in the actual sample of three different types of butyl xanthate containing surface water, domestic sewage, and industrial wastewater
After the spiked analysis, the recoveries were 87.2~103%, 90.5~99.0%, 88.8~96.0%, and the recovery rate was final.
Value. 93.4 ± 12.6%, 93.9 ± 6.8%, 92.1 ± 6.2%.
12 Quality Assurance and Quality Control
12.1 Make at least one blank for each batch of samples, and recalibrate the instrument zero after each analysis of 20 samples.
12.2 Each batch of samples should be subjected to a 10% parallel sample analysis, and the relative deviation of the measurement results should be controlled to less than 10%.
12.3 Each batch of samples should be subjected to 10% standard analysis, and the recovery rate should be controlled between 80% and 110%.
12.4 A calibration curve should be drawn for each batch of samples. In general, the correlation coefficient of the calibration curve should be above 0.999.
413 Waste treatment
The discarded standard solution of butyl xanthogen should be stored in a centralized manner and entrusted to a qualified unit for treatment.
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