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Limitation requirements of toxic and harmful substance in fertilizers
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GB 38400-2019: PDF in English GB 38400-2019
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 65.080
G 20
Limitation requirements of toxic and harmful
substance in fertilizers
ISSUED ON: DECEMBER 17, 2019
IMPLEMENTED ON: JULY 01, 2020
Issued by: State Administration for Market Regulation;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Terms and definitions ... 5
4 Requirements ... 6
5 Test method ... 8
6 Inspection rules ... 9
Appendix A (Normative) Terrestrial plant growth test ... 10
Appendix B (Normative) Determination of total nickel, total cobalt, total
vanadium, total antimony, total thallium in fertilizers Inductively coupled plasma
emission spectrometry ... 20
Appendix C (Informative) Species for plant testing ... 25
Appendix D (Informative) Examples of defining suitable growth conditions for
specific species in terrestrial plant growth tests ... 26
References ... 27
Limitation requirements of toxic and harmful
substance in fertilizers
1 Scope
This standard specifies the limit requirements, test methods, inspection rules
for toxic and harmful substances in fertilizers.
This standard applies to commercial fertilizers produced by various processes.
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) are applicable to this standard.
GB/T 2441.2 Determination of urea - Part 2: Biuret content -
Spectrophotometric method
GB 5085.1 Identification standards for hazardous wastes - Identification for
corrosivity
GB 5085.2 Identification standards for hazardous wastes - Screening test
for acute toxicity
GB 5085.3 Identification standards for hazardous wastes - Identification for
extraction toxicity
GB 5085.4 Identification standards for hazardous wastes - Identification for
ignitability
GB 5085.5 Identification standards for hazardous wastes - Identification for
reactivity
GB 5085.6 Identification standards for hazardous wastes - Identification for
toxic substance content
GB/T 8170-2008 Rules of rounding off for numerical values & expression
and judgement of limiting values
GB/T 19524.1 Determination of fecal coliforms in fertilizers
5 Test method
5.1 Corrosion identification
It is performed according to GB 5085.1.
5.2 Acute toxicity identification
It is performed according to GB 5085.2.
5.3 Identification of leaching toxicity
It is performed according to GB 5085.3.
5.4 Identification of flammability
It is performed according to GB 5085.4.
5.5 Identification of reactivity
It is performed according to GB 5085.5.
5.6 Identification of toxic substance content
It is performed according to GB 5085.6.
5.7 Total cadmium, total mercury, total arsenic, total lead, total chromium
It is performed according to GB/T 23349 or ISO 17318; GB/T 23349 is used as
the arbitration method.
5.8 Total nickel, total cobalt, total vanadium, total antimony, total thallium
It is performed according to Appendix B.
5.9 Biuret
It is performed according to GB/T 22924 or GB/T 2441.2 or ISO 18643; GB/T
22924 is used as the arbitration method.
5.10 Benzo[a]pyrene
It is performed according to GB/T 32952.
5.11 Total petroleum hydrocarbons
It is performed according to GB 5085.6.
5.12 Total phthalates
Appendix A
(Normative)
Terrestrial plant growth test
A.1 Test substance information
The test substance information includes but is not limited to: water solubility,
vapor pressure, structural formula, solubility in organic solvents, n-
octanol/water partition coefficient, absorption behavior, purity, stability in water
and light, results of biodegradation tests .
A.2 Introduction to test
A.2.1 Test purpose
Used to evaluate the potential toxic effects of solid and liquid chemicals in the
soil on plant seedlings and early growth after one-time application.
A.2.2 Test principle
This Appendix is used to evaluate the effects of applying the test substance in
the soil (or other suitable soil substrate) on the emergence of seedlings and the
early growth of higher plants. The seeds are planted in the soil treated with the
test product and evaluated within 14 d ~ 21 d after the emergence rate of the
control group reaches 50%. The end-point measurement is the visible
emergence rate, the dry weight of the seedling (or fresh weight), in some cases
the height of the seedling; it shall also evaluate the harmful effects visible on
different parts of the plant. These measurements and observations are
compared with untreated controls.
According to the possible exposure pathways, the test product is mixed into the
soil (or possible artificial soil substrate) or sprayed on the soil surface. These
pathways shall represent the potential exposure pathways of chemicals as
accurately as possible. When the soil is mixed, a large amount of loose soil is
mixed first, then it is put in a pot, the selected plant seeds are planted into the
soil. When applying the pesticide on the surface, put the soil in the pot first,
plant the seeds, then spray the pesticide. The test system (control and treated
soil and seeds) is placed in an environment suitable for plant growth.
This Appendix can determine the dose-response curve according to the
purpose of the study, or a single dose/ratio as a limit test. If the single-dose/ratio
test exceeds a certain level of toxicity (for example, the observed effect is higher
than x%), a range screening test is required to determine the upper and lower
toxicity limits; then a multiple-dose test is performed to generate a dose-
response curve. Appropriate statistical analysis methods are used to analyze
the test substance is not a plant protection product, the artificial substrate can
be used to replace the natural soil for the test. The matrix used shall contain
inert substances, to reduce interaction with the test product, solvent carrier or
both. Quartz sand, mineral wire and glass beads (such as: 0.35 mm ~ 0.85 mm
in diameter) that have been washed with acid are suitable inert substances,
which can reduce the absorption of the test product and ensure that the test
product reaches the seedlings through the root absorption as much as possible.
Unsuitable substrates include vermiculite, perlite or other highly absorbent
materials. The nutrients needed for plant growth shall be provided, to ensure
that the plants are not stressed by nutrient deficiency, which can be evaluated
by chemical analysis or visible evaluation of control plants.
A.4.2 Test plants
The selection of plant species shall consider its taxonomic diversity in the plant
kingdom, its distribution characteristics, the specific life history of the species,
the regional differences in natural distribution, including the following
characteristics:
- Having uniform seeds, obtained from reliable standard seed sources, can
produce continuous, reliable and consistent germination, as well as
consistent seedling growth;
- Plants shall be suitable for testing in the laboratory; it may obtain reliable
and reproducible results in and between laboratories;
- The sensitivity of the species used shall be consistent with the plant's
response to environmental exposure;
- The selected species have been used in some previous toxicity tests,
meanwhile their use in such as herbicide bioassays, heavy metal screening,
salinity or mineral stress tests or plant-related research shows that they are
sensitive to a wide variety of stimuli;
- Be able to adapt to the growth conditions in the test method;
- Meet the test validity standard.
The number of species used in the test is determined according to the relevant
management requirements. The species used in the plant test in Appendix C
are for reference.
A.4.3 Application of test article
The test product shall be applied to an appropriate carrier (such as: water,
acetone, ethanol, polyethylene glycol, gum Arabic, sand). It can also be tested
with formulations containing active ingredients and various additives.
A.4.6 Verification of the concentration/ratio of the test substance
The concentration shall be verified by appropriate analytical methods. For
soluble substances, verification of all concentrations can be confirmed by
analyzing the highest concentration used for gradual dilution. Use calibration
equipment (such as: calibration glassware for analysis, calibration spray
equipment) for stepwise dilution. For substances that are insoluble in water,
analyze the amount added to the soil. If it wants to prove the homogeneity of
the test product in the soil, it is necessary to conduct a soil analysis.
A.4.7 Test conditions
The test conditions shall be similar to the normal growth conditions of the test
species and varieties. The emergent plants shall be placed in a controlled
climate incubator, artificial climate box or greenhouse for gardening operations
to maintain normal growth. When using growth equipment, ensure that the
plants grow normally and compare with the control group. It shall record such
parameters as the temperature, relative humidity, carbon dioxide concentration,
light (illuminance, wavelength, photosynthetically active radiation)/photoperiod,
average irrigation volume and other parameters including condition control and
sufficient frequency (e.g. daily); the greenhouse temperature is controlled
through ventilation, heating and / or refrigeration system. The following
conditions are generally recommended for greenhouse tests:
- Temperature: (22 ± 10) °C;
- Relative humidity: (70 ± 25)%;
- Photoperiod: At least 16 h illumination;
- Illuminance: (24850 ± 3550) lx. If the illuminance drops below 14200 lx and
the wavelength is 400 nm ~ 700 nm, except for some species need to
reduce the illuminance, additional illumination is required.
During the test, the environmental conditions shall be monitored and recorded.
The container used in the test shall be a non-porous plastic or glass container,
a tray or dish shall be placed under the container. Containers shall be
repositioned regularly to reduce plant growth differences (because the test
conditions of the growth facilities are different). The container shall be large
enough to ensure normal growth.
In order to maintain good plant vitality, it can add soil nutrient solution. Judge
the need and timing of adding nutrient solution by observing the control plants.
It is recommended to water it from the bottom of the test container (for example,
use glass fiber filament).
For test plant species and test products, specific growth conditions are suitable
whether general chemicals have phytotoxic properties, the 1000 mg/kg dry soil
is usually used as the maximum dose.
A.4.8.3 Pre-test
Before conducting a formal multi-concentration dose-response study, it is
necessary to conduct a preliminary test to determine the dose range. The
concentration interval of the pre-test shall be wide (such as: 0.1 mg/kg, 1.0
mg/kg, 10 mg/kg, 100 mg/kg, 1000 mg/kg dry soil). The concentration of crop
protection products shall be determined according to the recommended or
maximum use concentration or application rate, such as 1/100, 1/10, 1/1 of the
recommended/maximum concentration or application ratio.
A.4.8.4 Multiple concentration/ratio test
The purpose of the multi-concentration/ratio test is to establish a dose-response
relationship and determine the germination rate, the ECx or ERx value of the
biomass and/or the observable effect compared with the untreated control
group.
The number and spacing of the test concentration/ratio shall be sufficient to
produce a credible dose-response relationship and regression linear equation
and an estimated ECx or ERx value. The number of selected concentrations
shall be at least five geometric levels plus the control; the two adjacent
concentration gradients shall not exceed 3 geometric levels. Each treatment
and control have at least four parallels; the total number of seeds shall be at
least 20. For some plants with low germination rate or plants with diversified
growth characteristics, increase the number of parallels to improve statistical
power.
A.4.8.5 Observation
During the observation period, that is, within 14 d ~ 21 d after the emergence
rate of the control (solvent control) reached 50%, regularly (at least 1 week, if
possible, daily) observe whether the plant emerges and there is visible plant
poisoning death. At the end of the test, record the emergence rate, the biomass
of surviving plants and the visible toxic effects in different parts of the plant. The
latter includes morphological abnormalities of emerging seedlings, growth
retardation, withering, discoloration, death, effects on plant development. The
final biomass is completed by measuring the average dry weight of the final
surviving plants. The plants above the soil surface are harvested and dried at
60 °C to a constant mass. It can also choose to use fresh weight as the final
biomass. If there are special requirements, the seedling height can be used as
another key indicator. A unified scoring system can be used to score visible
injuries to evaluate observable toxicity action.
results graphs and summaries. It usually includes the following:
a) Test product:
- Chemical identification data, characteristics of related substances (if
possible, the partition coefficient lgPOW of n-octanol/water, water
solubility, vapor pressure, environmental fate and behavior information);
- The preparation details of the test solution and the verification of the test
concentration.
b) Test plant species:
- Detailed information of the test organism: Species/subspecies, plant
family, scientific name and common name, source and history as
detailed as possible (i.e.: provider's name, germination rate, seed size
level, batch number, year of production or selected growing season,
budding stage level), viability, etc.;
- The number of monocot and dicot species tested;
- Reasons for choosing this type;
- Description of seed storage, handling and maintenance.
c) Test conditions:
- Test facilities (e.g. growth chamber, artificial climate chamber and room
temperature);
- Description of the test system (e.g. container diameter, container
material and soil volume);
- Soil characteristics (soil texture or type: soil particle distribution and
classification, physical and chemical characteristics, including organic
matter content, organic carbon content, pH value);
- Preparation of soil/substrate (such as soil, artificial soil, sand and others)
before the test;
- If nutrient solution is used, formula description;
- Application of the test product: application method, equipment, exposure
load and volume (including chemical verification, calibration method),
description of environmental conditions during application;
- Growth conditions: Illumination, photoperiod, maximum/minimum
temperature, watering schedule and method, fertilization;
Appendix B
(Normative)
Determination of total nickel, total cobalt, total vanadium, total
antimony, total thallium in fertilizers -- Inductively coupled plasma
emission spectrometry
Warning - The hydrochloric acid used in this Appendix is corrosive, the
nitric acid is corrosive and oxidizing, so the test personnel shall take
appropriate protection. This Appendix does not indicate all possible
security issues. The user is responsible for taking appropriate safety and
health measures and ensuring compliance with the conditions stipulated
by relevant national laws and regulations.
B.1 Method summary
The total nickel, total cobalt, total vanadium, total antimony, total thallium in the
specimen are digested and extracted with aqua regia, determined by inductively
coupled plasma emission spectrometry. When manganese and other elements
interfere with the determination, the total thallium is determined using aqua
regia sample; after the methyl isobutyl ketone is extracted and enriched, the
extract is evaporated to dryness, the residue is digested with nitric acid, then it
is determined by the inductively coupled plasma emission spectrometry.
B.2 Reagents
B.2.1 Nitric acid: Pure superior grade.
B.2.2 10% nitric acid solution: 1 volume of nitric acid is mixed with 9 volumes
of water.
B.2.3 Hydrochloric acid: Pure superior grade.
B.2.4 Hydrochloric acid solution: 1 + 1.
B.2.5 Potassium iodide-ascorbic acid solution: Weigh 30 g of potassium iodide
and 20 g of ascorbic acid in a beaker; add water to dissolve; transfer to a 100
mL volumetric flask; use ultrapure water to dilute it; mix it uniformly.
B.2.6 Methyl isobutyl ketone: Analytically pure.
B.2.7 Standard stock solution of nickel, cobalt, vanadium, antimony, thallium:
1.000 g/L, certified standard material.
B.2.8 High purity argon: Content ≥ 99.999%.
Add 4 mL of methyl isobutyl ketone each according to the same operation.
Continue 2 more extractions. Combine the organic phase. Please the
beaker on a boiling water bath to evaporate to dryness. Add 5 mL of nitric
acid to the beaker. Heat and digest on a hot plate and evaporate until the
solution volume is less than 1 mL (the solution cannot be evaporated to
dryness). Cool to room temperature. Transfer to a 10 mL volumetric flask.
Make it reach to the volume. Shake well. Prepare for use. If the test
solution is turbid, filter it before measurement;
b) Remove the watch glass slightly to continue heating. When the solution is
about 10 mL, remove it. Cool it down. Transfer to a 50 mL volumetric flask.
Make its volume reach to the mark. Perform dry filtering. Discard the first
10 mL filtrate. Accurately pipet 20 mL of the filtrate into a 50 mL
colorimetric tube. Add 3 mL of potassium iodide-ascorbic acid solution.
Shake well. Add 5 mL of methyl isobutyl ketone. Shake and extract for 2
minutes. After standing for 15 minutes, use a dropper to carefully remove
most of the organic phase in a 50 mL beaker. According to the same
operation, add 4 mL of methyl isobutyl ketone and continue to extract 2
times. Combine the organic phases and place the beaker on a boiling
water bath to evaporate to dryness. Add 5 mL of nitric acid to the beaker.
Heat and digest on a hot plate and evaporate until the volume of the
solution is less than 1 mL (the solution cannot be evaporated to dryness).
Cool to room temperature. Transfer to a 10 mL volumetric flask. Make its
volume reach to the mark. Shake well. Prepare for use. If the test solution
is turbid, filter it before measurement.
B.4.3 Preparation of blank solution
Except that no specimen is added, the other steps are the same as the
preparation of the specimen solution.
B.4.4 Preparation of working standard solution
Take an appropriate amount of standard stock solution of each element. Dilute
it step by step and use 10% nitric acid solution (B.2.2) to make it reach to the
volume. Prepare the mixed ion standard solution series according to Table B.1.
Appendix D
(Informative)
Examples of defining suitable growth conditions for specific
species in terrestrial plant growth tests
The following conditions are suitable for the following 10 crop species to be
tested in an incubator:
- Carbon dioxide’s volume fraction: 350 × 10-6 ± 50 × 10-6;
- Relative humidity: The relative humidity in the light cycle is about (70 ± 5)%,
the relative humidity in the dark cycle is about (90 ± 5)%;
- Temperature: 25 °C ± 3 °C during the day, 20 °C ± 3 °C at night;
- Photoperiod: 16 h light/8 h dark, light wavelength is 700 nm;
- Illumination: 24850 lx ± 3550 lx, at the top of test incubator.
The 10 crop species are:
- Tomato (Solanum lycopersicon, Solanum);
- Cucumber (Cucumi ssativus, Cucumber);
- Lactuca sativa (Lactuca sativa, Lactuca);
- Soybean (Glycine max, soybean);
- Cabbage (Brassica oleracea var. capitata, Brassica);
- Carrot (Daucus carota, Daucus);
- Oats (Avena sativa);
- Ryegrass (Lolium perenne, Lolium);
- Corn (Zea mays);
- Onion (Allium cepa).
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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