GB 29518-2013Diesel engines NOx reduction agent -- Aqueous urea solution (AUS 32) (English PDF)
柴油发动机氮氧化物还原剂 尿素水溶液(AUS 32)
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Issued by
General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China
Level / Type
National · Mandatory
Issue date
May 7, 2013
Implementation date
July 1, 2013
Scope
GB 29518-2013 is the English-translated version of 柴油发动机氮氧化物还原剂 尿素水溶液(AUS 32).
GB 29518-2013 — This standard specifies a diesel engine NOx reduction agent --- aqueous urea solution (AUS32) terms and definitions, identification technology to Sum test methods, inspection rules, marking, packaging, transportation and storage, and make a recommendation to the requirements of filling interface products. This standard applies to diesel selective catalytic reduction of nitrogen oxides with a reducing agent system --- aqueous urea solution (AUS32).
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Document preview — GB 29518-2013
National Standard of the People's Republic of China
- ICS
- 71.100.99
- Classification
- G 71
Issued by: General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China
Contents
- 1 Scope1
- 2 Normative References1
- Terms and definitions 13
- Identification 24
- 5 technical requirements and test methods2
- 6 Inspection Rules3
- 7 signs, packaging, transportation and storage3
- 8 filling Interface4
- Determination of urea content of Annex A (normative) in AUS32 (TN method)5
- Determination of alkalinity AUS32 (normative) Appendix B8
- Annex C (normative) AUS32 biuret assay11
- Determination of Annex D (normative) aldehydes of AUS3215
- Annex E (normative) AUS32 of insolubles content (gravimetric method)18
Foreword
This standard in Chapters 4 and 5 are mandatory, the rest are recommended.
This standard was drafted in accordance with rules GB/T 1.1-2009 given.
This standard uses redrafted modified method using ISO 22241-1.2006 "Diesel engine NOx reduction agent AUS32 1
Part. Quality Requirements ", ISO 22241-2.2006" Diesel engine AUS32 reducing the nitrogen oxides - Part 2. Test Method "and
ISO 22241-3.2008 "Diesel engine AUS32 reducing the nitrogen oxides - Part 3. handling, transport and storage."
This standard and ISO 22241-1.2006, ISO 22241-2.2006 and ISO 22241-3.2008 has more adjustment compared to the previous structure, attached
M record listed in this standard and ISO 22241-1.2006, ISO 22241-2.2006 and ISO 22241-3.2008 Number of control clauses
List.
This standard and ISO 22241-1.2006, ISO 22241-2. there is a technical difference compared to 2008.2006 and ISO 22241-3
Appendix N given in the corresponding technical Differences in the list.
This standard was proposed by the Ministry of Environmental Protection of the People's Republic of China.
This standard petroleum products by the National Standardization Technical Committee Technical Committee petroleum fuels and lubricants and lubricant (SAC /
TC280/SC1) centralized.
Drafted by. China Petrochemical Sales Co., Ltd. North China Branch, China Environmental Science Research Institute, China Petroleum & Chemical shares have
Lubricating Oil Company Limited, China Environmental Science Research Institute, China National Petroleum Marketing Company, China Petroleum Lanzhou lubricant research and development centers,
Sichuan Meifeng Chemical Co., Ltd.
1 Scope
This standard specifies a diesel engine NOx reduction agent --- aqueous urea solution (AUS32) terms and definitions, identification technology to
Sum test methods, inspection rules, marking, packaging, transportation and storage, and make a recommendation to the requirements of filling interface products.
This standard applies to diesel selective catalytic reduction of nitrogen oxides with a reducing agent system --- aqueous urea solution (AUS32).
2 Normative references
The following documents for the application of this document is essential. For dated references, only applies to the version dated paper
Pieces. For undated references, the latest edition (including any amendments) applies to this document.
Preparation GB/T 601 standard titration solution Chemicals
GB/T 614 General Method Chemicals refractive index determination (GB/T 614-2006, ISO 6353-1. 1982, NEQ)
GB/T 1884 Density of crude oil and liquid petroleum products laboratory assay (densitometer method) (GB/T 1884-2000, eqvISO
3675.1998)
GB/T 1885 Petroleum Measurement Tables (GB/T 1885-1998, eqvISO 91-2.1991)
GB/T 6682 for analytical laboratory use specifications and test methods (GB/T 6682-2008, ISO 3696. 1987, MOD)
SH/T 0604 Crude petroleum and petroleum products densitometry (U-shaped vibrating tube method) (SH/T 0604-2000, eqvISO 12185.1996)
Petroleum products ISO 4259 Test Method Determination of precision data (Petroleumproducts-Determinationand
applicationofprecisiondatainrelationtomethodsoftest)
Determination of free formaldehyde content of sodium sulfite titration (Binders ISO 9020 Paints and varnishes amine resin binder
forpaintsandvarnishes-Determinationoffree-formaldehydecontentofaminoresins-Sodiumsulfite
titrimetricmethod)
3 Terms and Definitions
The following terms and definitions apply to this document.
3.1
Selective catalytic reduction system selectivecatalyticreductionsystem; SCR
Installed in a diesel engine exhaust system, by injecting the reducing agent, nitrogen oxides in the exhaust gas catalytically reduced to nitrogen and water in a catalytic
Conversion means.
3.2
AUS32 dedicated urea ureaforAUS32
It contains only industrially produced urea, free of aldehydes and other trace substances biuret, ammonia and water (e.g., anti-caking agent), sulfur and vulcanization
, Chloride, nitrate and other compounds.
Note. For the above-mentioned contaminants, will have influence in the urea production process, and to strictly control the content of the test method, as used in agricultural production
Urea typically contains the compound.
3.3
Water purewater
With a single distillation, deionization, reverse osmosis or ultrafiltration, etc. The method of preparation of the third grade water GB/T 6682 provisions.
3.4
--- NOx reduction agent aqueous urea solution (AUS32) NOxreductionagent-Aqueousureasolution (AUS32)
Not containing any other additives (e.g., 3.2 shown) in pure AUS32 dedicated formulated together with the urea aqueous solution which urine
Su content of 32.5% (mass fraction), and meet the technical requirements specified in Chapter 5, referred to AUS32.
Note. the tracer in accordance with Table 1 may be used as an additive.
4 logo
Shall have the following markings on the charging pump and the container AUS32 compliance with this standard.
AUS32 GB 29518
5 technical requirements and test methods
Technical requirements and test methods for reducing nitrogen oxides in diesel engines --- aqueous urea solution (AUS32) shown in Table 1.
Table 1 --- diesel engine NOx reduction agent aqueous urea solution (AUS32) technical requirements and test methods
Project Quality Index Test Method
Urea content a (mass fraction) /% 31.8 33.2 Appendix Ad ~
Density b (20 °C) / (kg/m3) 1087.0 ~ 1093.0 SH/T 0604e
Refractive index c20nD 1.3814 ~ 1.3843 GB/T 614
Impurities
Alkalinity (in terms NH3) (mass fraction)/not more than 0.2%
Biuret (mass fraction)/not more than 0.3%
Aldehydes (in terms HCHO)/(mg/kg) no greater than 5
Insolubles/(mg/kg) not more than 20
Phosphate (in terms PO4)/(mg/kg) not greater than 0.5
Ca/(mg/kg) not greater than 0.5
Fe/(mg/kg) not greater than 0.5
Cu/(mg/kg) not more than 0.2
Zn/(mg/kg) not more than 0.2
Cr/(mg/kg) not more than 0.2
Ni/(mg/kg) not more than 0.2
Al/(mg/kg) not greater than 0.5
Mg/(mg/kg) not greater than 0.5
Sodium/(mg/kg) not greater than 0.5
K/(mg/kg) not greater than 0.5
Appendix B
Appendix C
Appendix D
Appendix E
Appendix F
Appendix G
Reference spectrum is consistent with the consistency confirmation Appendix H
Note. If you need to add a tracer to AUS32, we should ensure that the tracer does not affect the AUS32 meet the technical requirements in this table, it will not hurt
SCR systems.
a target value of 32.5% (mass fraction).
b target 1090.0kg/m3.
c target 1.3829.
Deduction of ammonia from nitrogen d is calculated.
e can be used GB/T 1884 and GB/T 1885, when the result of objections to SH/T 0604 arbitration method.
6 Inspection Rules
6.1 Test items and classification
This test is divided into product type test and factory inspection.
6.1.1 factory inspection
Factory inspection, including batches of the factory inspection and factory inspection cycle.
Delivery lot inspection items urea content, density, alkalinity, biuret.
When this product is the raw material and process conditions can affect product quality did not happen changes, factory inspection project cycle. aldehydes, phosphates, not
Solubles, refractive index, consistency confirmation, calcium, iron, copper, zinc, chromium, nickel, aluminum, magnesium, sodium, potassium content, tested once a month.
6.1.2 Type inspection
Type test items for all the items specified in Chapter 5.
Type test in the following cases.
a) production of new products or product type identification;
b) sources of raw materials or manufacturing process variations;
c) factory inspection results and the last type inspection results are quite different.
6.2 Batch
In the starting material, the same process conditions, the product tank or a jar each production batch.
6.3 Sampling
Sampling in accordance with Appendix I, the sample should include a reservation of an amount of samples for future reference.
6.4 determine the rules
The results of factory inspection when all meet the technical requirements in Table 1, and then determine whether the product is qualified.
6.5 Review criteria
If the result of factory inspection fails to meet the requirements specified in Table 1, in accordance with the provisions of 6.3 from the same batch of product re-drawn double
Times the sample be retested for the failed project. If the review the results still do not meet the targets, it is determined that the product failed.
7 signs, packaging, transportation and storage
7.1 marks
Costumes AUS32 containers should be clearly marked, it should include at least the following.
a) product name, packaging specifications, product standard number;
Date of manufacture b) products;
c) manufacturer's name, address, contact details;
d) rain, sun, storage temperature (-5 °C ~ 25 °C), up flag.
7.2 Packaging
Packaging material shall not affect the quality of AUS32, packaging materials should be selected in accordance with the provisions of Appendix J of.
7.3 Transportation and storage
Appendix J, in accordance with transport and storage.
8 filling Interface
Referring to Appendices Appendix K and L are predetermined.
Appendix A
(Normative)
Determination of urea content AUS32 (TN method)
A.1 Scope
This annex specifies a method for measuring the total nitrogen content of urea AUS32 method.
This method is suitable for detecting the urea solution in the urea content 30.0% to 35.0% (mass fraction).
A.2 Summary of Method
Samples high temperature combustion in an oxygen stream, nitrogen in the sample completely converted to nitrogen oxides. The generated interference component by a suitable absorbent
Removal of the nitrogen oxides are reduced to molecular nitrogen quantified after a thermal conductivity detector. Urea nitrogen content was determined by deducting from the total nitrogen reduction in diurea
Calculated.
A.3 instruments and equipment
A.3.1 automatic azotometer
Automatic Azotometer combustion.
A.3.2 Analytical balance
A sense of the amount of 0.0001g.
A.3.3 aids
Example.
---tweezers;
Trace --- blunt spatula;
--- pipette, from a fixed or variable size to 1000µL capacity 10µL pipette;
--- commonly used laboratory glassware.
A.4 reagents and materials
A.4.1 Water
In line with GB/T 6682 in two water requirement.
A.4.2 accelerant and other supplies
The selection azotometer used. The following examples are for reference only, container or other material may be used as needed.
Example.
--- tin capsules or the like sample container;
--- nitrogen-free oxidant, such as sucrose, cellulose;
--- nitrogen-liquid absorbent, such as magnesium oxide.
A.4.3 nitrogen Standards
Preferred materials certification standards, such as ethylenediaminetetraacetic acid (ethylenediaminetetraaceticacid, EDTA), and nicotinamide
(Nicotinicacidamide), may also be used high purity low biuret urea content (e.g., analytical pure urea crystals or urea),
Or equipment manufacturers recommendations or other similar reference materials provided.
A.4.4 oxygen
Purity of not less than 99.995%.
A.4.5 other gases
Depending on the requirements Azotometer selection.
A.5 analysis step
A.5.1 sample preparation
Samples should be completely dissolved, crystals can not be urea. If necessary, the sample may be heated to no more than 40 °C.
A.5.2 standard curve plotted
The requirements azotometer be used, according to the procedure A.5.4 to establish a standard curve.
A.5.3 working state testing equipment and standard curve
With a suitable reference material testing instrument conditions and the standard curve, preferably urea certified standard solutions. Inspection frequency
Depending on the use required azotometer may be.
A.5.4 Determination
Weighed sample is placed in line with a certain quality requirements azotometer suitable container (such as a tin capsule) in. The sample size of the sample shall ensure that its nitrogen content
In the middle range of the standard curve.
With approximately three times the amount of the oxidant (e.g., no nitrogen cellulose) and the liquid absorbent (such as magnesium oxide).
When a liquid sample delivery system, sample volume not less than 100µL. The sample mass calculated SH/T 0604 obtained density
get.
Enter the required data (e.g., quality, sample type) to azotometer (or computer) in. The measured amount of sample into the analyzer and start
combustion.
Each sample was subjected to at least three determinations.
Calculation and results expressed A.6
A.6.1 calculation results
First, calculate the standard curve should drift to correct a result of analysis by measuring the blank reading. Then use the instrument that comes with the program
To the standard calibration curve.
If the relative standard deviation of the test results (RSD) of greater than 1%, will have to re-test the samples.
Calculating the average, with at least three samples of a nitrogen content of the urea content of the test results according to formula (A.1) is calculated.
wU = 2.1438 × (wN-F × wBi) (A.1)
Where.
wU --- urea content (mass fraction),%;
wN --- average nitrogen content (mass fraction), two decimals,%;
--- F. Biuret factor into nitrogen (0.4076);
Appendix C WBI --- the concentration of the biuret assay (mass fraction)%.
A.6.2 The results indicate
To the arithmetic mean of three independent determination results do measurement results. After calculation reserved to one decimal place, in%.
A.7 precision
Table A.1.
Table A.1 precision
Urea content (mass fraction) wU /% Repeatability r /% Reproducibility R /%
30.0 - 35.0 0.4 1.0
A.8 Test report
The test report shall include at least the following.
a) The test samples of the described type, and;
b) a reference to this standard;
c) test results;
d) using the deviation of that particular operation;
e) date of the test.
Appendix B
(Normative)
Determination of alkalinity AUS32
B.1 Scope
This annex specifies measurement AUS32 alkalinity (as NH3 basis), measured in the range of 0.10% to 0.50% (mass fraction).
B.2 Methods Summary
Weighed amount of sample was added 100mL of water, with 0.01mol/L of hydrochloric acid standard solution was titrated to the end point (pH 5.7), and then the count
Samples alkalinity (as NH3 basis) calculated.
B.3 instruments and equipment
B.3.1 analytical balance. a sense of the amount of 0.0001g.
B.3.2 pH meter. measurement sensitivity 0.01pH, with glass pH electrode.
B.3.3 magnetic stirrer.
B.3.4 150mL tall beaker.
B.3.5 100mL graduated cylinder.
B.3.6 automatic titrator.
B.3.7 Burette. capacity 25mL, indexing is 0.1mL.
B.3.8 pipette. After verification 10mL pipette.
B.4 reagents and materials
B.4.1 water
In line with GB/T 6682 water three requirements.
B.4.2 standard hydrochloric acid solution
According to the procedure specified in GB/T 601 is formulated in a concentration of [c (HCl)] = 0.1mol/L hydrochloric acid standard solution.
B.4.3 buffer solution
Chosen according to the requirements of a pH meter. Generally 4.008,8.00 and 9.184.
Note. be used is selected according to different requirements of different instrumentation calibration standard buffer solution.
B.5 analysis step
B.5.1 pH meter calibration
With a pH of 4.008 and a pH standard buffer solution of 9.180 potentiometer function check to ensure the normal. a pH of 8.00 standard
Quasi buffer solution for daily inspection potentiometer.
B.5.2 0.01mol/L hydrochloric acid standard titration solution formulation
Accurately pipette the calibrated amount of 10mL 0.1mol/L hydrochloric acid standard titration solution, a 100mL volumetric flask, washed with water
Diluted to the mark, to give 0.01mol/L of hydrochloric acid standard titration solution.
B.5.3 preliminary measurements
1g samples were taken, accurate to 0.05g, the sample was placed into 150mL beaker was added 100mL of water. With 0.01mol/L of
The standard solution of hydrochloric acid solution was titrated to pH 5.7.
Calculating the ammonia content, the ammonia content in the sample according to the determined number of samples as shown in Table B.1 sample, to the nearest 0.05g.
Table B.1 sample volume
Ammonia content /% 0.02 0.05 0.1 0.2 0.5
Sample volume/g 10 5 2 1
B.5.4 measurement
Based on the results of preliminary experiments homogeneous mass mS weighed sample, accurate to 0.05g, placed in a beaker filled with 150mL 100mL water.
With 0.01mol/L of hydrochloric acid standard titration solution with stirring at a normal speed titrated to pH 7.5, and then slowly titrated to pH 5.7.
Calculation and results expressed B.6
B.6.1 calculation results
Alkalinity (as NH3 basis) content, according to equation (B.1) is calculated.
w (NH3) =
V × c × M
mS × 1000 ×
100 (B.1)
Where.
W (NH3) --- Alkalinity (in terms NH3) (mass fraction),%;
V --- volume of standard solution of hydrochloric acid consumed in titration, in milliliters (mL);
C --- hydrochloric acid standard titrant concentration in mol per liter (mol/L);
--- M ammonia molar mass in grams per mole (g/mol), M = 17.03;
--- mass mS sample in grams (g).
B.6.2 results indicate
In the arithmetic mean of test results of two test as a final result, data retention to 0.01% (mass fraction).
B.7 precision
Table B.2.
Table B.2 Precision
Alkali content (mass fraction) w (NH3) /% Repeatability r /% Reproducibility R /%
0.1 ~ 0.5 0.01 0.2 × x
Note. x is the average of two test results.
B.8 Test report
The report shall include at least the following.
a) The test samples of the described type, and;
b) a reference to this standard;
c) test results;
d) using the deviation of that particular operation;
e) date of the test.
Appendix C
(Normative)
Determination of biuret AUS32
C.1 Scope
This annex specifies determined by spectrophotometry AUS32 biuret content, scope biuret content is reduced to 0.1%
0.5% (mass fraction).
C.2 Method Summary
In an alkaline solution of potassium sodium tartrate, biuret is reacted with divalent copper produce a purple compound, the compound in wavelength
Absorption peak at 550nm. The purple compound Absorbance at a wavelength spectrophotometer at 550nm with. Biuret labeled with
Plotted standard curve standard solution, and then the absorbance of the sample on the standard curve concentration reduction diurea.
C.3 instruments and equipment
C.3.1 analytical balance. a sense of the amount of 0.001g.
C.3.2 vacuum filtration apparatus. Pore Size 0.45µm.
C.3.3 spectrophotometer. it can be used to determine the wavelength of 550nm, 50mm of the cuvette.
C.3.4 volumetric flask. Certificated 1000mL, 250mL, 50mL volumetric flask.
C.3.5 water bath. thermostatically at 30 °C ± 1 °C.
C.3.6 pipette. 2mL, 5mL, 10mL, 20mL pipette.
C.3.7 rotary evaporator.
C.4 reagents and materials
C.4.1 water
In line with GB/T 6682 water three requirements. Boiled prior to use to remove carbon dioxide.
C.4.2 saturated potassium carbonate solution
C.4.3 copper sulfate solution
15g of CuSO4 · 5H2O was dissolved in the carbon dioxide-free water, and transferred to a 1000mL volumetric flask to volume with water.
C.4.4 alkaline sodium potassium tartrate solution
The 40gNaOH dissolved in 500mL water. After cooling, 50g of sodium potassium tartrate (KNaC4H4O6 · 4H2O), stirred
Dissolved, transferred to a 1000mL volumetric flask, add water to the mark. Use After standing 1d.
C.4.5 biuret standard solution, 0.8mg/mL
Biuret before use should be dried for 3h in an oven at 105 °C. The biuret 800mg was dissolved in carbon dioxide-free water and dilute
To 1000mL. It can also be purchased through accredited commercial products.
Biuret can be purified in the following manner.
--- 50g of biuret were added to a concentration of 25% ammonia solution 500mL, stirred for 15min;
--- filtered, washed with ammonia-free water after rinsing and drying;
--- was dissolved in ethanol (10g/L), filtered, and heated to a low temperature so that 1/4 of the original volume of concentrate;
After cooling to 5 °C --- filtration;
--- dried in a vacuum dryer at 80 deg.] C;
--- check purity by step C.5.5 luminometer.
Recrystallization in ethanol should be repeated until no longer be purified so far.
C.5 analysis step
C.5.1 possible causes of interference
Spectrophotometric test solution required to be transparent, so the sample first through 0.45µm filter means to obtain a clear solution.
Ammonia to form a divalent copper 550nm light energy absorption of a colored compound. This method does not only exceed strip 500mg/kg in the ammonia content
Piece applicable.
In order to remove the ammonia exceeds 500mg/kg, the 1L flask, 50g of sample is placed on a rotary evaporator, was added 15mL saturated carbon
Potassium silicate solution, the rotational speed is 60r/min, a temperature of 40 °C, 1h was evaporated under vacuum to a final volume of about a pressure of 2kPa ~ 3kPa
20mL. And then transferred to a 250mL volumetric flask to volume.
Draw the standard curve C.5.2
Were pipetted 0mL, 2mL, 5mL, 10mL, 15mL, 20mL and 25mL biuret standard solution 50mL capacity to 7
Bottle, were added to the mixture of water total volume of about 25mL. After each addition, was added with stirring 10mL alkaline solution of potassium sodium tartrate
10mL copper sulfate solution and the flask placed in 30 °C ± 1 °C water bath and allowed to stand 15min.
After removing the flask was cooled to room temperature, diluted with water to the mark. 50mm thickness of the cuvette, with water as a reference solution,
Absorbance was measured at a wavelength of 550nm.
Corrected absorbance of the blank solution. In biuret content standard solution as the abscissa, the ordinate is the absorbance corresponding to establish
standard curve line. Standard curve should have good linearity in the concentration range.
C.5.3 correction factor calculation
According to the formula (C.1) calculating a correction factor.
F =
i = 1
mBi, i
i = 1
(E1, i-E2)
= 61.6
i = 1
(E1, i-E2)
(C.1)
Where.
--- correction factor F., Milligrams (mg);
MBI, biuret i --- i th sample mass, in milligrams (mg);
E1, i --- i absorbance of the sample;
E2 --- blank test absorbance.
Standard Curve and Determination of the correction factor should be repeated every year, and archiving.
twenty one
C.5.4 Coefficients of calculation
Coefficient should be measured once a week.
Of 10mL biuret standard solution (containing biuret 8mg), is detected by the analysis step. Then according to the formula (C.2) calculation of the optical
coefficient.
FD = 8 (E1-E2)
(C.2)
Where.
--- the FD-optic coefficient, in milligrams (mg);
--- E1 standard solution absorbance (average of two experiments);
E2 --- blank test absorbance.
Coefficient of variation should be within ± 5% of the correction factor. When the sample was measured, the coefficient is used.
C.5.5 measure
100g ...
END: Draft Version (GB 29518-2013)
......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — all pages — is available in the English PDF.
Referenced standards
Normative references
- GB/T 601Chemical Reagent - Preparations of Standard Volumetric Solutions
- GB/T 614Chemical reagent - General method for the determination of refractive index
- GB/T 614-2006Chemical reagent - General method for the determination of refractive index
- GB/T 6682Water for analytical laboratory use - Specification and test methods
- GB/T 6682-2008Water for analytical laboratory use - Specification and test methods
ISO 6353 · GB/T 1884 · GB/T 1884-2000 · GB/T 1885 · GB/T 1885-1998 · ISO 3696 · ISO 4259 · ISO 9020
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