GB/T 15063-2020 PDF in English
GB/T 15063-2020 (GB/T15063-2020, GBT 15063-2020, GBT15063-2020)
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Compound fertilizer
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| GB 15063-2009 | English | 85 |
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[GB/T 15063-2009] Compound fertilizer (Complex fertilizer)
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| GB 15063-2001 | English | 399 |
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| GB 15063-1994 | English | 559 |
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GB/T 15063-2020: PDF in English (GBT 15063-2020) GB/T 15063-2020
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 65.080
G 21
Replacing GB/T 15063-2009
Compound fertilizer
复合肥料
ISSUED ON: NOVEMBER 19, 2020
IMPLEMENTED ON: JUNE 01, 2021
Issued by: State Administration for Market Regulation;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative references ... 5
3 Terms and definitions... 6
4 Technical requirements ... 7
5 Sampling ... 8
6 Test methods ... 10
7 Inspection rules ... 13
8 Identification and quality certificate ... 14
9 Packaging, transportation, storage ... 15
Appendix A (Normative) Determination of available phosphorus content in compound
fertilizers - Quinoline phosphomolybdate gravimetric method ... 17
Appendix B (Normative) Determination of chloride ion content in compound fertilizers
- Automatic potentiometric titration ... 21
Appendix C (Normative) Determination of available calcium and available magnesium
content in compound fertilizer - Plasma emission spectrometry ... 24
Compound fertilizer
1 Scope
This standard specifies the terms and definitions, technical requirements, sampling, test
methods, inspection rules, marking and quality certificates, packaging, transportation,
storage of compound fertilizers.
This standard applies to compound fertilizers (including ternary or binary solid
fertilizers, which use nitrogen, phosphorus, potassium as basic nutrients, under various
names). This standard does not apply to compound fertilizer products, such as
monoammonium phosphate and diammonium phosphate.
2 Normative references
The following documents are essential to the application of this document. For the dated
documents, only the versions with the dates indicated are applicable to this document;
for the undated documents, only the latest version (including all the amendments) is
applicable to this standard.
GB/T 3597 Fertilizer - Determination of nitrate nitrogen content - Nitron gravimetric
method
GB/T 6274 Fertilizers and soil conditioners - Vocabulary
GB/T 6679 General rules for sampling solid chemical products
GB/T 8170 Rules of rounding off for numerical values & expression and judgement
of limiting values
GB/T 8569 Packing of solid chemical fertilizers
GB/T 8571 Preparation of laboratory samples for compound fertilizers
GB/T 8572-2010 Determination of total nitrogen content for compound fertilizers
titrimetric method after distillation
GB/T 8573 Determination of available phosphorus content for compound fertilizers
GB/T 8574 Determination of potassium content for compound fertilizers -
Potassium tetraphenylborate gravimetric method
5.2 Sample reduction
Quickly mix the collected aggregate sample uniformly. Use a divider or quartering
method, to reduce the sample to about 1 kg. Then divide it into two parts, which are
divided into two clean and dry glass or plastic bottles with ground stoppers (the quality
inspection department of the manufacturer can use a clean and dry plastic Ziplock bag,
to hold the sample). Seal and label it. Indicate the name of the manufacturer, product
name, batch number or production date, sampling date and the name of the sampler.
One bottle is used for product inspection; the other bottle is retained for two month, for
future reference.
6 Test methods
6.1 General provisions
Except for appearance and particle size, make parallel determinations of two sets of
samples. The reagents, solutions, water, which is used in this standard, shall comply
with the provisions of HG/T 2843, when the specifications and preparation methods are
not specified.
6.2 Visual inspection
Use the sample in 5.2, to make inspection visually.
6.3 Total nutrients
6.3.1 Determination of total nitrogen content
6.3.1.1 Method 1: Post-distillation titration (arbitration method)
It is carried out, in accordance with GB/T 8572.
6.3.1.2 Method 2: Automatic analyzer method
After the specimen is prepared, according to the provisions of GB/T 8571 (if the sample
is difficult to pulverize, it can be ground, until it passes through a 1.00 mm aperture test
sieve). It is determined, according to GB/T 22923.
6.3.1.3 Method 3: Dumas combustion method
It is carried out, in accordance with 3.2 of NY/T 1977-2010.
6.3.2 Determination of available phosphorus content and calculation of the
percentage of water-soluble phosphorus in available phosphorus
6.3.2.1 Method 1: Quinoline phosphomolybdate gravimetric method (Arbitration
method)
It is carried out, in accordance with Appendix A.
6.3.2.2 Method 2: Quinoline phosphomolybdate gravimetric method or plasma
emission spectrometry
It is carried out, in accordance with GB/T 8573.
6.3.2.3 Method 3: Automatic analyzer method
After the specimen is prepared, according to the provisions of GB/T 8571 (if the sample
is difficult to pulverize, it can be ground, until it passes through a 1.00 mm aperture test
sieve). It is determined according to GB/T 22923.
6.3.3 Determination of potassium content
6.3.3.1 Method 1: Potassium tetraphenylborate gravimetric method (Arbitration
method)
It is carried out, in accordance with GB/T 8574.
6.3.3.2 Method 2: Automatic analyzer method
After the specimen is prepared, according to the provisions of GB/T 8571 (if the sample
is difficult to pulverize, it can be ground until, it passes through a 1.00 mm aperture test
sieve). It is determined according to GB/T 22923.
6.3.3.3 Method 3: Plasma emission spectrometry
Prepare the specimen solution, according to 4.3.2 of NY/T 2540-2014. Then it is
determined, in accordance with 5.3 of NY/T 2540-2014.
6.3.4 Calculation of total nutrients
Total nutrients are the sum of total nitrogen, available phosphorus, potassium content.
6.4 Determination of nitrate nitrogen content
6.4.1 Method 1: Nitrogen reagent gravimetric method (arbitration method)
After the specimen is prepared, according to the provisions of GB/T 8571 (if the sample
is difficult to pulverize, it can be ground, until it passes through a 1.00 mm aperture test
sieve). Then it is determined, according to GB/T 3597.
6.4.2 Method 2: Automatic analyzer method
After the specimen is prepared, according to the provisions of GB/T 8571 (if the sample
is difficult to pulverize, it can be ground, until it passes through a 1.00 mm aperture test
sieve). Then it is determined, according to GB/T 22923.
7.3.1 The qualification of the product quality indicators, in this standard, shall be
determined, by the "rounding-off value comparison method", in GB/T 8170.
7.3.2 Manufacturers shall carry out the exit-factory inspection and type inspection,
according to the requirements of this standard. When all the inspection items meet the
requirements of this standard, the batch of products is judged to be qualified.
7.3.3 If one of the indicators, in the results of the exit-factory inspection or type
inspection, which is conducted by the manufacturer, does not meet the requirements of
this standard, double amount of samples shall be taken from the same batch of
packaging containers, for inspection. In the re-inspection results, even if there is one
indicator does not meet the requirements of this standard, the batch of products is
judged to be unqualified.
8 Identification and quality certificate
8.1 If the product contains nitrate nitrogen, it shall be marked with "nitrate nitrogen",
on the packaging container.
8.2 When the products, which use the citrate-soluble phosphate fertilizers, such as
calcium-magnesium-phosphate fertilizers, as the basic fertilizer, they shall be marked
as "citrate-soluble phosphorus", in a prominent position of the packaging container.
8.3 For products whose mass fraction of chloride ions is greater than 3.0%, it shall,
according to the "mass fraction of chloride ions" required in 4.2, clearly mark the
Chinese characters "chlorine-contained (low chlorine)", "chlorine-contained (medium
chlorine)", "chlorine-contained (high chlorine)", in prominent positions of the
packaging container, rather than “chlorine", “Cl-contained” or “Cl”, etc. For products,
which are marked with “Chlorine-contained”, it shall not have pictures of chlorine-
sensitive crops on the packaging container, nor shall it have markings such as
"potassium sulfate (type)", "potassium nitrate (type)", "sulfur group", "nitrosulfur
group", which may easily lead users to misunderstand that the product does not contain
chlorine. For products, which have the marking of "chlorine-contained (high chlorine)",
it shall be marked of the warning words that "high chlorine content; improper use will
cause damage to crop and soil".
8.4 For the products, which contain amide nitrogen (urea nitrogen), it shall be marked
with the following warning words, in a prominent position on the packaging container:
"Containing biuret; improper use will cause damage to crops". For products, which are
not marked with this warning, the inspection and testing agency may select a method
for measuring the total nitrogen content for detection and determination, based on the
fact that the product does not contain amide nitrogen (urea nitrogen).
8.5 If medium elements and (or) trace elements are added, the content of each single
element can be indicated separately, according to the medium elements and (or) trace
elements (both are calculated as elemental elements); the content of medium elements
and trace elements shall not be included in the total nutrients. When the content of
available calcium and available magnesium, in a single medium element, is less than
1.0%, the total sulfur content is less than 2.0%, the content of a single trace element is
less than 0.02%, it shall not be marked.
8.6 There shall be warnings, precautions for use, etc., on the outer packaging container
of the product. Some product information, such as production date or batch number,
certificate of conformity, instructions for use, can be marked with easily identifiable
QR codes or barcodes.
8.7 If fertilizer additives, other than the requirements of this standard, are marked on
the product packaging, it shall mark the name, function, content, corresponding testing
method standards of the additives, on the packaging container.
8.8 The marking of nutrient content shall be labelled on the basis of the total material;
the material in the packaging container shall not be separated and labelled separately.
8.9 The net content of each bag shall be marked with a single value, such as 50 kg.
8.10 Each batch of qualified exit-factory products shall be accompanied by a quality
certificate, which includes: manufacturer's name, address, product name, batch number
or date of manufacture, total nutrients, formula or main nutrient content, chloride ion
content, biuret content, this standard number, as well as the content that shall be marked
according to laws and regulations. For the products, which use the citrate-soluble
phosphate fertilizers, such as calcium-magnesium phosphate fertilizers, as the basis, it
shall be marked as "citrate-soluble phosphorus"; meanwhile, it shall indicate whether
they are "nitrate nitrogen", "urea nitrogen", "organic nitrogen". Non-exit-factory
inspection items are marked with the test results of the latest type inspection.
8.11 The rest shall be implemented, in accordance with the provisions of GB 18382.
9 Packaging, transportation, storage
9.1 The product is packaged, by the materials that meet the requirements of GB/T 8569.
The packaging specifications are 1000 kg, 50 kg, 40 kg, 25 kg; the allowable range of
the net content of each bag is (1000 ± 10) kg, (50 ± 0.5) kg, (40 ± 0.4) kg, (25 ± 0.25)
kg; the average net content of each bag of each batch of products shall not be less than
1000 kg, 50.0 kg, 40.0 kg, 25.0 kg. Other packaging specifications, which are agreed
upon by both parties in the contract, can also be used.
9.2 When there are additives in the product, within the stated net content range of each
bag, they shall be mixed with the raw materials evenly; they shall not be put into the
packaging bag, in the form of small packages.
9.3 On the premise of complying with the provisions of GB/T 8569, it should use the
Appendix A
(Normative)
Determination of available phosphorus content in compound fertilizers -
Quinoline phosphomolybdate gravimetric method
A.1 Principle
Water-soluble phosphorus is extracted, by grinding with water or ultrasonically. Use an
alkaline solution of disodium ethylenediaminetetraacetate (EDTA), which has a pH
value between 12.0 and 12.5, to heat and boil it, to extract the available phosphorus in
the compound fertilizer. The extract is boiled with nitric acid solution, for more than 10
min, to completely convert the non-orthophosphate in the test solution into
orthophosphate. In acidic medium, the content of water-soluble phosphorus and
available phosphorus is determined, by quinoline phosphomolybdate gravimetric
method.
A.2 Reagents or materials
A.2.1 Sodium hydroxide solution: 200 g/L.
A.2.2 Disodium ethylenediaminetetraacetate (EDTA) alkaline solution: Weigh 37.5 g
of disodium EDTA. Dissolve it in 1000 mL of water. Mix well. Adjust the pH value to
12.0 ~ 12.5, by sodium hydroxide solution (A.2.1), before use.
A.2.3 Nitric acid solution: 1 + 1.
A.2.4 Quinmolybdenum limonene reagent.
A.3 Instruments and equipment
A.3.1 Usually laboratory instruments are used.
A.3.2 Ultrasonic cleaning instrument: It can control the temperature (30 ± 2) °C.
A.3.3 Electric heating constant temperature drying oven: The temperature can be
controlled at (180 ± 2) °C.
A.3.4 Glass crucible filter: No.4, 30 mL.
A.4 Sample
A.4.1 Specimen preparation
It is carried out, according to the provisions of GB/T 8571 (if the sample is difficult to
pulverize, it can be ground to pass the 1.00 mm aperture test sieve).
A.4.2 Weighing of specimen
Weigh the sample, which contains 100 mg ~ 180 mg of phosphorus pentoxide, from
A.4.1, accurate to 0.0002 g.
A.5 Test procedure
A.5.1 Extraction of water-soluble phosphorus
A.5.1.1 Extraction method 1 (grinding by adding water): Weigh the sample, according
to the requirements of A.4.2. Place it in a 75 mL porcelain evaporating dish. Add 25 mL
water to grind it. Pour the clear liquid into the 250 mL volumetric flask, which was pre-
filled with 5 mL of nitric acid solution. Continue to grind with water three times, using
25 mL of water each time. Then transfer the water-insoluble matter to the filter paper.
Use water to wash the water-insoluble matter, until the solution in the volumetric flask
is about 200 mL. Finally, use water to dilute it to the mark. Mix well, to obtain the
solution A, which is used for the determination of water-soluble phosphorus.
A.5.1.2 Extraction method 2 (ultrasonic extraction): Weigh the sample, according to the
requirements of A.4.2. Place it in a 250 mL volumetric flask. Add 150 mL of water.
Shake to make the sample evenly dispersed. Add the stopper tightly. Place the
volumetric flask in the ultrasonic cleaner, to extract it for 10 min (the liquid level of the
ultrasonic cleaner shall be higher than the liquid level of the volumetric flask). Use
water to dilute it to the mark. Mix well. Perform dry filtration. Discard the initial part
of the filtrate, to obtain the solution B, which is used for the determination of water-
soluble phosphorus.
Note: The method A.5.1.1 is used to extract water-soluble phosphorus, during arbitration.
A.5.2 Extraction of available phosphorus
Weigh the sample, according to the requirements of A.4.2. Place it in a 400 mL beaker.
Add 150 mL of EDTA alkaline solution. Cover with a watch glass. Place it on an electric
hot plate, to heat for 15 min. Remove it. Cool it to room temperature. Quantitatively
transfer it to a 250 mL volumetric flask. Use water to dilute it to the mark. Mix well.
Perform dry filtration. Discard the initial part of the filtrate, to obtain the solution C,
which is used for the determination of available phosphorus.
A.5.3 Determination of water-soluble phosphorus
Use a single-marked pipette, to pipette 25 mL of solution A or solution B. Transfer it
into a 400 mL high beaker. Add 20 mL of nitric acid solution. Use water to dilute it to
100 mL. Add a glass rod and stir evenly. Cover with a watch glass. Heat on a hot plate
for at least 10 min. Remove it. Use a small amount of water, to rinse the watch glass
and the inner wall of the beaker. Add 35 mL of quinolybdenum limonene reagent. Cover
Appendix B
(Normative)
Determination of chloride ion content in compound fertilizers - Automatic
potentiometric titration
B.1 Principle
Boil with water, to extract the chloride ion in the sample. Use the silver electrode as the
indicator electrode. Use the silver nitrate standard titration solution, to titrate the
chloride ion in the test solution. Use the sharp change of potential of the automatic
potentiometric titrator, to determine the reaction end point. Use the consumed volume
of silver nitrate standard titration solution, to calculate the chloride ion content.
B.2 Reagents or materials
B.2.1 Silver nitrate solution [c(AgNO3) = 0.01 mol/L]: Weigh 1.7 g of silver nitrate.
Dissolve it in water. Add water to dilute it to 1000 mL. Store it in a brown bottle.
B.2.2 Chloride ion standard solution (1 mg/mL): Accurately weigh 1.6487 g of standard
sodium chloride, which was dried at 270 °C ~ 300 °C for 4 h, in a 100 mL beaker. Use
a small amount of water to dissolve it. Transfer it into a 1000 mL volumetric flask. Use
water to dilute it to the mark. Mix well. Store it in a plastic bottle.
B.3 Instruments and equipment
B.3.1 General laboratory instruments.
B.3.2 Automatic potentiometric titrator, which is equipped with silver electrodes.
B.4 Sample
It is carried out, according to the provisions of GB/T 8571 (if the sample is difficult to
pulverize, it can be ground to pass the 1.00 mm aperture test sieve).
B.5 Test procedure
B.5.1 Calibration of silver nitrate solution
Accurately pipette 3.0 mL of chloride ion standard solution, into the titration cup. Add
water, until the liquid level covers the electrode. Then calibrate it. The relative
difference, between the two calibration values, shall not be greater than 0.5%.
B.5.2 Preparation of specimen solution
Appendix C
(Normative)
Determination of available calcium and available magnesium content in
compound fertilizer - Plasma emission spectrometry
C.1 Principle
Use citric acid solution at (30 ± 2) °C constant temperature, to perform oscillation or
ultrasonic to extract available calcium and available magnesium in compound fertilizer.
The calcium and magnesium in specimen solution are atomized and excited to high
energy state, in plasma emission (ICP) light source. When the atoms in the high-energy
state transition to the ground state, it generates electromagnetic radiation with
characteristic wavelengths. The radiation intensity is proportional to the concentration
of calcium and magnesium atoms.
C.2 Reagents or materials
C.2.1 Citric acid solution (20 g/L): Weigh 20 g of citric acid, in a 1000 mL beaker. Add
water to dissolve it, to dilute it to 1000 mL. Mix well. Store it in a plastic bottle.
C.2.2 Calcium standard solution: ρ (Ca) = 1 mg/mL.
C.2.3 Magnesium standard solution: ρ (Mg) = 1 mg/mL.
C.2.4 High-purity argon.
C.3 Instruments and equipment
C.3.1 Laboratory instruments are usually used.
C.3.2 Constant temperature water bath oscillator: It can control the temperature at (30
± 2) °C.
C.3.3 Ultrasonic cleaning instrument: It can control the temperature at (30 ± 2) °C.
C.3.4 Plasma emission spectrometer.
C.4 Sample
It is carried out, according to the provisions of GB/T 8571 (if the sample is difficult to
pulverize, it can be ground to pass the 1.00 mm aperture test sieve).
C.5 Test procedure
C.5.1 Extraction of available calcium and available magnesium
C.5.1.1 Extraction method 1 (extraction by citric acid constant temperature oscillation):
Weigh 1 g ~ 2 g of sample (accurate to 0.0002 g) from C.4. Put it in a 250 mL volumetric
flask. Add 150 mL of citric acid solution. Shake it to make the specimen evenly
dispersed. Close the bottle stopper. Place it in a constant temperature water bath
oscillator, at (30 ± 2) °C. Perform oscillation extraction, at constant temperature for 1
h. Take it out. Cool it to room temperature. Use water to dilute it to the mark. Mix well.
Perform dry filtration. Discard the initial part of the filtrate, to obtain the solution D,
which is used for the determination of available calcium and available magnesium.
C.5.1.2 Extraction method 2 (extraction by citric acid ultrasonic): Weigh 1 g ~ 2 g of
sample (accurate to 0.0002 g) from C.4. Put it in a 250 mL volumetric flask. Add 150
mL of citric acid solution. Shake to make the sample disperse evenly. Close the stopper.
Place it in a (30 ± 2) °C ultrasonic cleaner, for constant temperature ultrasonic extraction,
for 10 minutes. Take it out. Cool it to room temperature. Use water to dilute it to the
mark. Mix well. Perform dry filtration. Discard the initial part of the filtrate, to obtain
the solution E, which is used for the determination of available calcium and available
magnesium.
C.5.2 Drawing of working curve
Draw 0 mL, 0.50 mL, 1.00 mL, 4.00 mL, 8.00 mL, 10.00 mL of calcium and magnesium
standard solutions, respectively, into six 100 mL volumetric flasks. Use water to dilute
it to the mark. Mix well. The mass concentrations of calcium and magnesium in this
standard series are 0 μg/mL, 5.0 μg/mL, 10.0 μg/mL, 40.0 μg/mL, 80.0 μg/mL, 100.0
μg/mL, respectively.
Before the measurement, according to the properties of the element to be measured and
the performance of the instrument, optimize the measurement conditions, such as argon
gas flow, observation height, video generator power, integration time. Then, use a
plasma emission spectrometer, to measure the radiation intensity of each standard
solution, at wavelengths of 317.933 nm (calcium) and 285.213 nm (magnesium). Take
the mass concentration of calcium and magnesium (μg/mL) of each standard solution
as the abscissa AND the corresponding radiation intensity as the ordinate, to draw the
working curve.
Note: The mass concentration of the standard curve can be adjusted, according to different
instrument sensitivities.
C.5.3 Determination
After specimen solution D or specimen solution E is directly or properly diluted, under
the same conditions as the standard series solutions, measure the radiation intensity of
calcium and magnesium. Check the corresponding mass concentrations of calcium and
magnesium (μg/mL), on the working curve.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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