NY/T 1447-2007 PDF English
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NY
AGRICULTURAL INDUSTRY STANDARD
ICS 65.120
B 46
Feed additive - Benzoic acid
Issued on. SEPTEMBER 14, 2007
Implemented on. DECEMBER 1, 2007
Issued by. Ministry of Agriculture of the People's Republic of China
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative references... 4
3 Requirements... 5
4 Test methods... 5
5 Inspection rules... 14
6 Marking, packaging, transport, storage and guarantee period... 15
Foreword
This Standard was proposed by Ministry of Agriculture of the People’s Republic of
China.
This Standard shall be under the jurisdiction of National Technical Committee on Feed
of Standardization Administration of China.
The drafting organizations of this Standard. Institute of Quality Standard and Testing
technology for Agro-products of CAAS, China National Feed Quality Supervision and
Testing Centre (Beijing).
The main drafters of this Standard. Song Rong, Li Lan, Tian Jing, Wang Peilong, Wang
Tong, Gao Sheng.
Feed additive – Benzoic acid
1 Scope
This Standard specifies the requirements, test methods, inspection rules, marking,
packaging, transport, storage and guarantee period of feed additive benzoic acid.
This Standard applies to feed additive benzoic acid which is made through catalytic
oxidation and purification using petroleum toluene as the raw material. This product is
mainly used as the agents for corrosion resistance, mould resistance and acidification
of feed.
Molecular formula. C7H6O2
Structural formula.
Relative molecular mass. 122.12 (based on the International Relative Atomic Mass
2001)
2 Normative references
The provisions in following documents become the provisions of this Standard through
reference in this Standard. For dated references, the subsequent amendments
(excluding corrigendum) or revisions do not apply to this Standard, however, parties
who reach an agreement based on this Standard are encouraged to study if the latest
versions of these documents are applicable. For undated references, the latest edition
of the referenced document applies.
GB/T 601, Chemical reagent – Preparations of standard volumetric solutions
GB/T 602, Chemical reagent – Preparations of standard solutions for impurity
determination
GB/T 603, Chemical reagent – Preparations of reagent solution for use in test
method
GB/T 606, Chemical reagent – General method for the determination of water –
Karl Fischer method
3 Requirements
3.1 Appearance and character
This product is white crystal, which has a slight odour of benzoin or benzaldehyde.
3.2 Specifications
4 Test methods
Unless specified otherwise, only reagents confirmed to be analytically pure and grade
3 water specified in GB/T 6682 are used in the analysis; standard volumetric solutions,
standard solutions for impurity determination and reagent solutions used in the
analysis shall be prepared as specified in GB/T 601, GB/T 602 and GB/T 603, unless
specified otherwise.
4.1 Identification test
4.1.1 Reagents
4.1.2 Analytical procedures
Weigh about 1 g of sample to dissolve in 20 mL of sodium hydroxide solution; add 1
drop of ferric trichloride solution to generate a reddish brown precipitation; then add
hydrochloric acid solution for acidification to separate out the precipitation.
4.2 Determination of benzoic acid content
4.2.1 Principle
Use neutral ethanol solution as the solvent and phenolphthalein as the indicator; use
sodium hydroxide standard volumetric solution to titrate sample; calculate the benzoic
acid content based on the consumption of sodium hydroxide standard volumetric
solution.
4.2.2 Reagents
4.2.2.1 95% ethanol.
4.2.3 Analytical procedures
Weigh about 0.25 g of dried sample (placed in a desiccator for 3 h), accurate to 0.0001
g; place in a conical flask; add 25 mL of neutral ethanol solution to dissolve; add 2
drops of phenolphthalein indicator solution; use sodium hydroxide standard volumetric
solution for titration until the test solution appears pink.
4.2.4 Result calculation
The content of benzoic acid W1, which is expressed as mass fraction (mg/kg), is
calculated according to Equation (1).
4.3 Melting point determination
As specified in GB/T 617.
4.4 Easy oxide test
4.4.1 Principle
The easy oxide in sample reacts with potassium permanganate; after reaction, it is the
end of reaction when the solution appears the pink colour of potassium permanganate
solution; use the volume of potassium permanganate standard volumetric solution
consumed to control the amount of easy oxide.
4.4.2 Reagents
4.4.2.1 Sulfuric acid.
4.4.2.2 Potassium permanganate standard volumetric solution. c(1/5kMnO4) = 0.02
mol/L.
4.4.3 Analytical procedures
Add 1.5 mL of sulfuric acid to 100 mL of water; add dropwise potassium permanganate
standard volumetric solution until pink while boiling; maintain for 30 without fading.
4.5 Determination of heavy metal (in terms of Pb) content
4.5.1 Principle
Use ethanol to dissolve sample; heavy metal and sodium sulfide generate a brown
sulfide; compare its colour with the reference solution under equal conditions.
4.5.2 Reagents
4.5.2.1 Ethanol.
4.5.2.2 Acetic acid solution. volume fraction 5%.
4.5.2.3 Sodium sulfide solution. 0.1 g/mL. Dissolve 1 g of sodium sulfide in 10 mL of
water; prepare immediately prior to use.
4.5.3 Analytical procedures
Weigh 1 g of sample, accurate to 0.001 g; place in a 50 mL colourimetric tube; add 20
mL of ethanol solution; add 2 mL of acetic acid solution; use water to add dropwise to
25 mL; mix up as the test solution.
Take another same colourimetric tube; add 1.0 mL of lead standard solution (4.5.2.5)
and 2 mL of acetic acid solution; use water to dilute to 25 mL as the standard
colourimetric solution.
Into the two colourimetric tubes, add 2 drops of sodium sulfide solution respectively;
mix up; after placing aside for 5 min, observe and compare the colour of the two tubes
of solution from above and side against a white background; the colour of the test
solution shall not be darker than that of the standard colourimetric solution.
4.6 Determination of arsenic (As) content
4.6.1 Principle
In an acidic solution, use potassium iodide and stannous chloride to reduce high
arsenic to trivalent arsenic; trivalent arsenic reacts with nascent hydrogen to generate
arsenic hydride gas; it forms brownish yellow arsenic stains on the mercury bromide
test paper; then compare with the standard arsenic stains.
4.6.2 Reagents
4.6.2.8 Lead acetate cotton.
4.6.2.9 Mercury bromide test paper.
4.6.3 Apparatus
Arsenic determination instrument.
4.6.4 Analytical procedures
Weigh 1 g of sample, accurate to 0.001 g; place in a 30 mL porcelain crucible; after
low-temperature carbonization to smokeless, transfer to a high-temperature furnace
for carbonization at 550°C for 3.5 ~ 4 h.
4.7 Determination of chloride (in terms of Cl) content
4.7.1 Principle
Sample contains organic chlorides (aromatic chlorides) and inorganic chlorides;
organic chlorides are converted into calcium chloride by addition of calcium carbonate
and burning at high temperature, before it is dissolved into the sample solution along
with inorganic chlorides. Under acidic conditions, chloride ion in the sample solution
reacts with silver nitrate solution to generate a silver chloride precipitation and the
turbidity generated shall not be greater than that of the standard turbidimetric solution.
4.7.2 Reagents
4.7.2.1 Calcium carbonate.
4.7.2.2 Nitric acid solution. 1 + 9.
4.7.2.3 Silver nitrate solution. 17 g/L.
4.7.2.4 Chloride (Cl) standard solution. 0.1 mg/mL.
4.7.3 Analytical procedures
Weigh about 0.5 g of sample and about 0.7 g of calcium carbonate, accurate to 0.001
g; place in a porcelain crucible; add a small amount of water to mix up; dry at 100°C ±
5°C to no obvious wet spots; burn at about 600°C for 10 min; add 20 mL of nitric acid
solution to dissolve residues; collect the filtrate in a 50 mL colourimetric tube; use 15
mL of water to wash insoluble substances; combine washings with filtrate; add water
to the scale of 50 mL as the test solution.
4.8 Water
Determine water content of sample using the method specified in GB/T 606.
4.9 Phthalic acid test
4.9.1 Principle
Dissolve sample in the mixed solution of methanol and 1% acetic acid; use the liquid
chromatography for quantitative analysis.
4.9.2 Reagents
4.9.2.1 Methanol.
4.9.2.2 Acetic acid solution. volume fraction 1%.
4.9.2.3 Mixed solution of methanol + 1% acetic acid = 2 + 3.
4.9.2.4 Phthalic acid standard stock solution, 100 μg/mL. weigh 10 mg of phthalic acid
standard substance; dissolve in 30 mL of methanol before adding 1% acetic acid
dropwise to 100 mL.
4.9.2.5 Phthalic acid standard working solution, 1.0 μg/mL. take 1.0 mL of phthalic acid
standard stock solution (4.9.2.4); add the mixed solution of methanol and 1% acetic
acid dropwise to 100 mL.
4.9.3 Apparatus
Liquid chromatograph, which is equipped with an ultraviolet detector.
4.9.4 Analytical procedures
Weigh 1 g of sample, accurate to 0.0001 g; dissolve in 20 mL of methanol before
adding acetic acid dropwise to 50 mL as the sample test solution. Take respectively 20
μL of phthalic acid standard working solution and sample test solution as sample.
4.9.5 Operating conditions for apparatus
Chromatographic column. C18 column, 4.6 mm × 250 mm.
Column temperature. 40°C.
Moving phase. mixed solution of methanol + 1% acetic acid = 3 + 7.
Determination wavelength. 228 nm.
Flow velocity. 1 mL/min.
4.9.6 Result calculation
The content of phthalic acid of sample W2, which is expressed as mass fraction (mg/kg),
is calculated in accordance with Equation (2).
5 Inspection rules
5.1 Inspection types
Product inspection includes exit-factory inspection and type inspection.
5.2 Batch and sampling
1,000 kg is deemed as an inspection batch. take 2% of the bag number of each batch
as sample, not less than 3 bags for a small batch. From the bags selected, use a
sampling tool to stretch ¾ into each bag and take not less than 100 g of sample.
5.3 Exit-factory inspection
5.3.1 Before delivery, exit-factory inspection shall be carried out for each batch;
products can only be delivered after they pass the inspection.
5.4 Type inspection
5.4.1 Type inspection shall be carried out in one of the following cases.
5.4.2 Inspection which is carried out for all the requirements specified in this Standard,
is type inspection.
5.4.3 Qualification criteria
First carry out exit-factory inspection for products to decide whether they are
acceptable; then carry out the other items of inspection for products which have passed
exit-factory inspection. If one of the other items fails, then the batch of products fails to
pass the inspection.
6 Marking, packaging, transport, storage and guarantee period
6.1 Marking
Package shall be provided with firm marks; the content of labelling shall be as specified
in GB 10648.
6.2 Packaging
Packaging bags shall be aluminium foil bags or composite plastic bags. Outer packing
is cardboard boxes. Each package shall enclose labels and product certificates.
6.4 Storage
Products shall be stored in a dark, cool, dry place and kept under airtight conditions.
6.5 Guarantee period
Under the specified storage conditions, the guarantee period is 24 months.
NY/T 1447-2007
NY
AGRICULTURAL INDUSTRY STANDARD
ICS 65.120
B 46
Feed additive - Benzoic acid
Issued on. SEPTEMBER 14, 2007
Implemented on. DECEMBER 1, 2007
Issued by. Ministry of Agriculture of the People's Republic of China
Table of Contents
Foreword... 3
1 Scope... 4
2 Normative references... 4
3 Requirements... 5
4 Test methods... 5
5 Inspection rules... 14
6 Marking, packaging, transport, storage and guarantee period... 15
Foreword
This Standard was proposed by Ministry of Agriculture of the People’s Republic of
China.
This Standard shall be under the jurisdiction of National Technical Committee on Feed
of Standardization Administration of China.
The drafting organizations of this Standard. Institute of Quality Standard and Testing
technology for Agro-products of CAAS, China National Feed Quality Supervision and
Testing Centre (Beijing).
The main drafters of this Standard. Song Rong, Li Lan, Tian Jing, Wang Peilong, Wang
Tong, Gao Sheng.
Feed additive – Benzoic acid
1 Scope
This Standard specifies the requirements, test methods, inspection rules, marking,
packaging, transport, storage and guarantee period of feed additive benzoic acid.
This Standard applies to feed additive benzoic acid which is made through catalytic
oxidation and purification using petroleum toluene as the raw material. This product is
mainly used as the agents for corrosion resistance, mould resistance and acidification
of feed.
Molecular formula. C7H6O2
Structural formula.
Relative molecular mass. 122.12 (based on the International Relative Atomic Mass
2001)
2 Normative references
The provisions in following documents become the provisions of this Standard through
reference in this Standard. For dated references, the subsequent amendments
(excluding corrigendum) or revisions do not apply to this Standard, however, parties
who reach an agreement based on this Standard are encouraged to study if the latest
versions of these documents are applicable. For undated references, the latest edition
of the referenced document applies.
GB/T 601, Chemical reagent – Preparations of standard volumetric solutions
GB/T 602, Chemical reagent – Preparations of standard solutions for impurity
determination
GB/T 603, Chemical reagent – Preparations of reagent solution for use in test
method
GB/T 606, Chemical reagent – General method for the determination of water –
Karl Fischer method
3 Requirements
3.1 Appearance and character
This product is white crystal, which has a slight odour of benzoin or benzaldehyde.
3.2 Specifications
4 Test methods
Unless specified otherwise, only reagents confirmed to be analytically pure and grade
3 water specified in GB/T 6682 are used in the analysis; standard volumetric solutions,
standard solutions for impurity determination and reagent solutions used in the
analysis shall be prepared as specified in GB/T 601, GB/T 602 and GB/T 603, unless
specified otherwise.
4.1 Identification test
4.1.1 Reagents
4.1.2 Analytical procedures
Weigh about 1 g of sample to dissolve in 20 mL of sodium hydroxide solution; add 1
drop of ferric trichloride solution to generate a reddish brown precipitation; then add
hydrochloric acid solution for acidification to separate out the precipitation.
4.2 Determination of benzoic acid content
4.2.1 Principle
Use neutral ethanol solution as the solvent and phenolphthalein as the indicator; use
sodium hydroxide standard volumetric solution to titrate sample; calculate the benzoic
acid content based on the consumption of sodium hydroxide standard volumetric
solution.
4.2.2 Reagents
4.2.2.1 95% ethanol.
4.2.3 Analytical procedures
Weigh about 0.25 g of dried sample (placed in a desiccator for 3 h), accurate to 0.0001
g; place in a conical flask; add 25 mL of neutral ethanol solution to dissolve; add 2
drops of phenolphthalein indicator solution; use sodium hydroxide standard volumetric
solution for titration until the test solution appears pink.
4.2.4 Result calculation
The content of benzoic acid W1, which is expressed as mass fraction (mg/kg), is
calculated according to Equation (1).
4.3 Melting point determination
As specified in GB/T 617.
4.4 Easy oxide test
4.4.1 Principle
The easy oxide in sample reacts with potassium permanganate; after reaction, it is the
end of reaction when the solution appears the pink colour of potassium permanganate
solution; use the volume of potassium permanganate standard volumetric solution
consumed to control the amount of easy oxide.
4.4.2 Reagents
4.4.2.1 Sulfuric acid.
4.4.2.2 Potassium permanganate standard volumetric solution. c(1/5kMnO4) = 0.02
mol/L.
4.4.3 Analytical procedures
Add 1.5 mL of sulfuric acid to 100 mL of water; add dropwise potassium permanganate
standard volumetric solution until pink while boiling; maintain for 30 without fading.
4.5 Determination of heavy metal (in terms of Pb) content
4.5.1 Principle
Use ethanol to dissolve sample; heavy metal and sodium sulfide generate a brown
sulfide; compare its colour with the reference solution under equal conditions.
4.5.2 Reagents
4.5.2.1 Ethanol.
4.5.2.2 Acetic acid solution. volume fraction 5%.
4.5.2.3 Sodium sulfide solution. 0.1 g/mL. Dissolve 1 g of sodium sulfide in 10 mL of
water; prepare immediately prior to use.
4.5.3 Analytical procedures
Weigh 1 g of sample, accurate to 0.001 g; place in a 50 mL colourimetric tube; add 20
mL of ethanol solution; add 2 mL of acetic acid solution; use water to add dropwise to
25 mL; mix up as the test solution.
Take another same colourimetric tube; add 1.0 mL of lead standard solution (4.5.2.5)
and 2 mL of acetic acid solution; use water to dilute to 25 mL as the standard
colourimetric solution.
Into the two colourimetric tubes, add 2 drops of sodium sulfide solution respectively;
mix up; after placing aside for 5 min, observe and compare the colour of the two tubes
of solution from above and side against a white background; the colour of the test
solution shall not be darker than that of the standard colourimetric solution.
4.6 Determination of arsenic (As) content
4.6.1 Principle
In an acidic solution, use potassium iodide and stannous chloride to reduce high
arsenic to trivalent arsenic; trivalent arsenic reacts with nascent hydrogen to generate
arsenic hydride gas; it forms brownish yellow arsenic stains on the mercury bromide
test paper; then compare with the standard arsenic stains.
4.6.2 Reagents
4.6.2.8 Lead acetate cotton.
4.6.2.9 Mercury bromide test paper.
4.6.3 Apparatus
Arsenic determination instrument.
4.6.4 Analytical procedures
Weigh 1 g of sample, accurate to 0.001 g; place in a 30 mL porcelain crucible; after
low-temperature carbonization to smokeless, transfer to a high-temperature furnace
for carbonization at 550°C for 3.5 ~ 4 h.
4.7 Determination of chloride (in terms of Cl) content
4.7.1 Principle
Sample contains organic chlorides (aromatic chlorides) and inorganic chlorides;
organic chlorides are converted into calcium chloride by addition of calcium carbonate
and burning at high temperature, before it is dissolved into the sample solution along
with inorganic chlorides. Under acidic conditions, chloride ion in the sample solution
reacts with silver nitrate solution to generate a silver chloride precipitation and the
turbidity generated shall not be greater than that of the standard turbidimetric solution.
4.7.2 Reagents
4.7.2.1 Calcium carbonate.
4.7.2.2 Nitric acid solution. 1 + 9.
4.7.2.3 Silver nitrate solution. 17 g/L.
4.7.2.4 Chloride (Cl) standard solution. 0.1 mg/mL.
4.7.3 Analytical procedures
Weigh about 0.5 g of sample and about 0.7 g of calcium carbonate, accurate to 0.001
g; place in a porcelain crucible; add a small amount of water to mix up; dry at 100°C ±
5°C to no obvious wet spots; burn at about 600°C for 10 min; add 20 mL of nitric acid
solution to dissolve residues; collect the filtrate in a 50 mL colourimetric tube; use 15
mL of water to wash insoluble substances; combine washings with filtrate; add water
to the scale of 50 mL as the test solution.
4.8 Water
Determine water content of sample using the method specified in GB/T 606.
4.9 Phthalic acid test
4.9.1 Principle
Dissolve sample in the mixed solution of methanol and 1% acetic acid; use the liquid
chromatography for quantitative analysis.
4.9.2 Reagents
4.9.2.1 Methanol.
4.9.2.2 Acetic acid solution. volume fraction 1%.
4.9.2.3 Mixed solution of methanol + 1% acetic acid = 2 + 3.
4.9.2.4 Phthalic acid standard stock solution, 100 μg/mL. weigh 10 mg of phthalic acid
standard substance; dissolve in 30 mL of methanol before adding 1% acetic acid
dropwise to 100 mL.
4.9.2.5 Phthalic acid standard working solution, 1.0 μg/mL. take 1.0 mL of phthalic acid
standard stock solution (4.9.2.4); add the mixed solution of methanol and 1% acetic
acid dropwise to 100 mL.
4.9.3 Apparatus
Liquid chromatograph, which is equipped with an ultraviolet detector.
4.9.4 Analytical procedures
Weigh 1 g of sample, accurate to 0.0001 g; dissolve in 20 mL of methanol before
adding acetic acid dropwise to 50 mL as the sample test solution. Take respectively 20
μL of phthalic acid standard working solution and sample test solution as sample.
4.9.5 Operating conditions for apparatus
Chromatographic column. C18 column, 4.6 mm × 250 mm.
Column temperature. 40°C.
Moving phase. mixed solution of methanol + 1% acetic acid = 3 + 7.
Determination wavelength. 228 nm.
Flow velocity. 1 mL/min.
4.9.6 Result calculation
The content of phthalic acid of sample W2, which is expressed as mass fraction (mg/kg),
is calculated in accordance with Equation (2).
5 Inspection rules
5.1 Inspection types
Product inspection includes exit-factory inspection and type inspection.
5.2 Batch and sampling
1,000 kg is deemed as an inspection batch. take 2% of the bag number of each batch
as sample, not less than 3 bags for a small batch. From the bags selected, use a
sampling tool to stretch ¾ into each bag and take not less than 100 g of sample.
5.3 Exit-factory inspection
5.3.1 Before delivery, exit-factory inspection shall be carried out for each batch;
products can only be delivered after they pass the inspection.
5.4 Type inspection
5.4.1 Type inspection shall be carried out in one of the following cases.
5.4.2 Inspection which is carried out for all the requirements specified in this Standard,
is type inspection.
5.4.3 Qualification criteria
First carry out exit-factory inspection for products to decide whether they are
acceptable; then carry out the other items of inspection for products which have passed
exit-factory inspection. If one of the other items fails, then the batch of products fails to
pass the inspection.
6 Marking, packaging, transport, storage and guarantee period
6.1 Marking
Package shall be provided with firm marks; the content of labelling shall be as specified
in GB 10648.
6.2 Packaging
Packaging bags shall be aluminium foil bags or composite plastic bags. Outer packing
is cardboard boxes. Each package shall enclose labels and product certificates.
6.4 Storage
Products shall be stored in a dark, cool, dry place and kept under airtight conditions.
6.5 Guarantee period
Under the specified storage conditions, the guarantee period is 24 months.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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