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Jointly Released by: Beidou Aerospace New Energy Science & Technology (Guangdong) Co., Ltd China Power & Pride New Energy Technology Co., Ltd CORPORATE STANDARD M15 Methanol Gasoline For Motor Vehicles QB/BD_DW·01182013 Authors: Mr. KUNG Kwong Ming, Mr. LIU Aiguo, Mr. SHEN Jianliang, Mr. GUO Yibin, Mr. LI Jialiang & Mr. XU Jianqiang Translated By: Mr. KUNG Kit Date of Release: 18 th April, 2013 Date of Implementation: 1 st May, 2013

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CORPORATE STANDARD

M15 Methanol Gasoline

For Motor Vehicles

QB/BD_DW·0118-2013

Authors: Mr. KUNG Kwong Ming, Mr. LIU Aiguo,

Mr. SHEN Jianliang, Mr. GUO Yibin,

Mr. LI Jialiang & Mr. XU Jianqiang

Translated By: Mr. KUNG Kit

Date of Release: 18th April, 2013

Date of Implementation: 1st May, 2013

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TABLE OF CONTENT

Preface ............................................................................................... 3

1. Scope ............................................................................................. 4

2. Normative References ....................................................................... 4

3. Terms and Definition ......................................................................... 6

4. Classification and Labeling ................................................................. 6

5. Requirements .................................................................................. 7

6. Testing Methods .............................................................................. 8

7. Inspection Regulation ........................................................................ 9

8. Signs, Packaging, Transportation and Storage ...................................... 10

9. Safety ............................................................................................ 10

10. Implementation ............................................................................. 10

Appendix A (Informative): Rapid Determination for Methanol Content of

Methanol Gasoline for Motor Vehicles .................................................... 11

Appendix B (Normative): Determination for Methanol Content of M15

Methanol Gasoline for Motor Vehicles (Gas Chromatography ..................... 13

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Preface This document is drafted with accordance to the regulations and standards of

“GB/T1.1-2009: Standardized Working Guidelines Part 1”.

(NOTE: Some contents of this document may involve patents. We, the issuing

organization, do not assume any responsibility for these patents.)

The standards in this document are first proposed by the Research &

Development Department of Beidou Aerospace New Energy Science &

Technology (Guangdong) Co., Ltd.

This document was first published in 2013.

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M15 Methanol Gasoline for Motor Vehicles

1. Scope

The standards regulate and specify the terms and definitions, classification and

labeling, requirements, testing methods, inspection regulations, signs,

packaging, transportation and storage for M15 methanol gasoline for motor

vehicles.

The standards apply to the production and testing methods of M15 methanol

gasoline used by internally ignited combustion engines.

2. Normative References

The following documents are essential for the application of this document.

(NOTE: For dated references, only the dated editions are applicable to this

document. For undated references, the latest editions (including any

amendments) apply to this document.)

GB 190 Packaging of dangerous goods standard signs

GB/T 259 Petroleum products – Determination of water-soluble acid

and alkali

GB/T 380 Petroleum products – Determination of sulfur content

(lamp method)

GB/T 503 Determination of gasoline octane number (MON)

GB/T 511 Petroleum products and additives - Determination of

mechanical impurities (gravimetric method)

GB/T 1792 Mercaptan sulfur distillate fuel assay (Potentiometric

titration)

GB/T 4756 Petroleum liquids hand sampling method

GB/T 5096 Petroleum products copper corrosion test

GB/T 5487 Determination of gasoline octane number (Research

method)

GB/T 6536 Petroleum products - Determination of distillation

GB/T 8017 Petroleum products - Determination of vapor pressure

(Reid method)

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GB/T 8018 Determination of oxidation stability of gasoline (Induction

period method)

GB/T 8019 Motor gasoline and aviation fuel gum assay (Jet

evaporation method)

GB/T 8020 Determination of lead content of gasoline (Atomic

absorption spectrometry)

GB/T 11132 Liquid petroleum products - Determination of

hydrocarbons (Fluorescent indicator adsorption method)

GB/T 11140 Petroleum products - Determination of sulfur (X-ray

spectroscopy)

GB 17930 Motor gasoline

SH 0164 Petroleum products, packaging, storage and delivery

acceptance rules

SH/T 0102 Lubricating oil and liquid fuels - Determination of copper

SH/T 0020 Determination of phosphorus content in gasoline

(Spectrophotometry)

SH/T 0174 Aromatics and light petroleum products mercaptan

qualitative test method

SH/T 0246 Light petroleum products Determination of water (Power

Law)

SH/T 0253 Light petroleum products - Determination of total sulfur

(Power Law)

SH/T 0663 Petrol certain alcohols and ethers assay (GC)

SH/T 0689 Light hydrocarbon fuel and other oil products -

Determination of total sulfur (UV fluorescence)

SH/T 0693 Aromatics content in gasoline Determination Act (GC)

SH/T 0711 Determination of manganese content in gasoline (Atomic

absorption spectrometry)

SH/T 0712 Iron content in gasoline Determination Act (Atomic

absorption spectrometry)

SH/T 0713 Determination car gasoline and aviation gasoline benzene

and toluene content (GC)

SH/T 0741 Gasoline Hydrocarbon Composition Determination

(Multidimensional gas chromatography)

SH/T 0742 Determination of sulfur content in gasoline (Energy

dispersive X-ray fluorescence spectrometry)

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3. Terms and Definition

The following terms and definitions apply to this document of standards:

3.1 Anti-knock index

Anti-knock index equals to one-half of the sum of the research octane number

(RON) and motor octane number (MON).

3.2 M15 methanol gasoline for motor vehicles

When gasoline components (either Class A or Class B) added with 14-16% of

the denatured methanol, is known as M15 methanol gasoline.

4. Classification and Labelling

4.1 Products Classification

M15 methanol gasoline for motor vehicles (IV*), with accordance to the

research octane number, is classified into 4 grades: 90#, 93#, 97# and 98#.

4.2 Products Labeling

Methanol gasoline for motor vehicles shall be labeled by the following symbols:

"M15/90 gasoline", "M15/93 gasoline", "M15/97 gasoline" and "M15/98

gasoline".

Remarks:

*The national 4th generation standard of P.R.China

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5. Requirements

The technological requirements for M15 methanol gasoline for motor vehicles

are shown in the below table:

Item Quality Indicator(s)

Testing Method(s) 90# 93# 97# 98#

Methanol Contenta(%) (14~16)% SH/T 0663

Antiknock

Index

(RON) ≥ 90 93 97 98 GB/T 5487

(RON+MON)/2 ≥ 85 88 Report Report GB/T 503、GB/T 5487

Lead Contentb(g/L ) ≤ 0.005 GB/T 8020

Distillation Range 10% Evaporation temp ℃ ≤ 60

GB/T 6536

50% Evaporation temp ℃ ≤ 100

90% Evaporation temp ℃ ≤ 190

Final boiling point ℃ ≤ 200

Residues %(v/v)≤ 2

Distillate Clear and transparent;

no phase separation

By observation

Saturated vapor

pressured(kPa)

1st Nov – 30th Apr ≤ 82 GB/T 8017、SH/T 0794

1st May – 31st Oct ≤ 70

Existent gum(mg/100mL)≤ 5 GB/T 8019

Induction period(min)≥ 480 GB/T 8018

Sulphur Contente (Mass fraction %)≤ 0.005 GB/T 380, GB/T 11140,

SH/T 0253, SH/T 0689

Mercaptan Dr. Experiment Passed SH/T 0174

Mercaptan sulfur content%

(Mass fraction) ≤

0.001 GB/T 1792

Copper corrosion(50℃,3h); grade ≤ 1 GB/T 5096

Water-soluble acid or alkali Nil GB/T 259

Mechanical impuritiesf Nil By observation, GB/T 511

Water Contentg(Mass fraction %) ≤ 0.10 SH/T 0246, GB/T 6283

Benzene Contenth(Volume fraction %) ≤ 1.0 SH/T 0693, SH/T 0713

Aromatic Contenti(Volume fraction %) ≤ 35 GB/T 11132, SH/T 0741

Olefin Content(Volume fraction %) ≤ 25 GB/T 11132, SH/T 0741

Manganese Contentj/(g/L) ≤ 0.002 SH/T 0711

Iron Contentk/(g/L) ≤ 0.01 SH/T 0712

Copper Contentl/(g/L) ≤ 0.010 SH/T 0102

Phosphorus Content /(g/L) ≤ 0.001 SH/T 0020

Phase anti-separation properties against low temperature

(-40℃,12h)

Clear and transparent;

no phase separation By observation

Phase anti-separation properties against water

(0.3% of water; oscillation for 3mins)

Clear and transparent; standing 8h with

no phase separation

By observation

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Remarks:

a) The lower limit of methanol content cannot be less than 14%.

b) No artificial addition

c) From the initial boiling point to the end point of the period, distillate phase separation is not allowed.

d) When there is objection, the results shall be justified based on GB/T 8017

e) When there is objection, the results shall be justified based on SH/T 0689

f) Injecting the sample into a 100mL glass cylinder for observation, it should be transparent without suspended mechanical

impurities and water settlement; when there is objection, the results shall be justified based on GB/T 511

g) When there is objection, the results shall be justified based on GB/T 6283

h) When there is objection, the results shall be justified based on SH/T 0713

i) For methanol gasoline over 97#, under the circumstance that the total amounts of olefins and aromatics remain unchanged,

the maximum value (volume fraction) of aromatics can be allowed to meet the value of Euro IV (or State IV), i.e. 35%; when

there is objection, the results shall be justified based on GB/T 11132

j) No artificial addition of manganese additives

k) No artificial addition of iron-containing additives

l) No artificial addition of copper-containing additives

Table.1: Corporate Standards for M15 methanol gasoline proposed by

Beidou Aerospace New Energy Science & Technology (Guangdong) Co., Ltd

6. Testing Methods

6.1 Phase anti-separation performance against low temperature

Samples shall be taken of each 200ml, and be dropped separately into two

250ml graduated cylinders with stoppers, and then be placed vertically into

refrigerator adjusted to -40℃ (allowable temperature difference ± 2℃ ).

Observations shall be made after 12 hours of placement.

6.2 Phase anti-separation performance against water

Samples shall be taken of each 200ml, and be dropped separately into two

250ml graduated cylinders with stoppers, vertically placed. 0.6mL of distilled

water shall be added into the containers respectively and then be oscillated for

about 3 minutes. Observations shall be made after 8 hours of placement at

room temperature.

6.3 Other tests

Other testing methods can be carried out as listed in Table 1.

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7. Inspection Regulations

7.1 Batches and sampling

7.1.1 Products manufactured from the same raw materials, formulation and

process conditions is classified as one product batch.

7.1.2 Sampling is done according to GB/T 4756. 4L of samples shall be taken

for inspection and reserve sample use.

7.2 Factory inspection

7.2.1 Products shall be examined and inspected by authorized quality

inspection departments with reference to standards of this document for

standard factory inspection and compliance testing. Qualified products shall be

issued with acceptable quality inspection reports before actual sales can

process.

7.2.2 Testing items shall be all the items listed in Table 1.

7.3 Type inspection

7.3.1 When one of the following conditions occurs, type inspection shall be

carried out:

a) When a new product type is under identification;

b) Any change of raw materials, formulation or processes;

c) Normal production (once a year);

d) Restoration of production after discontinuance;

e) Required type inspection by the national quality supervision and

inspection authority

7.3.2 In case any non-compliance is found in factory test with accordance to

Section 5 (Table 1), re-testing with double amounts of samples according to

the provisions of GB/T 4756. The product is determined failed if the re-test still

results any non-compliance with accordance to Section 5 (Table 1).

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8. Signs, Packaging, Transportation and Storage

8.1 According to GB 13690 and GB 12268, M15 methanol gasoline for

motor vehicles belongs to Class 3 flammable liquids and toxic substances. The

labeling, packaging, transportation, storage and delivery of products shall be

processed with accordance to the related requirements of SH 0164 and GB 190.

8.2 Significant parts of storage tanks and refueling equipment shall be

labeled correspondingly according to Section 4.2 of this document of standards.

9. Safety

9.1 The storage containers, transportation pipes, pumps, seals and

materials shall be applicable for methanol gasoline use.

9.2 Methanol gasoline is classified as Class 3 flammable liquids. The main

danger is flammable property with toxic nature. Safety management shall be

complied with the State safety administration regulations for hazardous

chemicals.

9.3 When handling and refueling methanol gasoline, volatile vapors shall

be avoided. The operator(s) shall make the appropriate protective measures in

order to avoid inhalation of harmful vapors.

9.4 Methanol gasoline is prohibited for oral contact, and shall be avoided

contact with skin. If skin or eyes are splashed on by methanol gasoline, the

contacted area shall be rinsed with plenty of water immediately. In case of

accidents, please seek medical attention promptly.

9.5 Methanol gasoline shall only be used as fuel in internally ignited

combustion engines. No other purpose is allowed.

10. Implementation

This document of standards is released on 18th April, 2013, effective from 1st

May, 2013.

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Appendix A (Informative):

Rapid Determination for Methanol Content of Methanol

Gasoline for Motor Vehicles

A.1 Scope

The standards regulate the rapid determination for methanol content of

methanol gasoline for motor vehicles, where the method applies to methanol

gasoline with methanol content ranging from 4% - 32%.

A.2 Reference

GB/T 6536 Petroleum products - Determination of distillation.

A.3 Method Summary

According to GB/T 6536, 100 mL of sample shall be taken for distillation,

distillate produced before reaching 75oC shall be collected by 100mL cylinder

with stopper. The volume of the distillate shall be recorded, and then added

with 20mL of distilled water and the mixture shall be shaken into oil-water

phases. After standing 30 minutes, the gasoline volume shall be recorded for

calculating the methanol content.

A.4 Instruments

A.4.1 Distillation tester in line with GB/T 6536

A.4.2 100mL cylinder with stopper; calibrated by 0.5 mL

A.5 Reagent

Distilled water

A.6 Testing procedures

A.6.1 100mL of sample (accurate to 0.5mL; the same below) shall be

collected by 100mL measuring cylinder with stopper.

A.6.2 The sample shall be transferred to a distillation flask, allow distillation

according to GB/T 6536. The distillate is collected using plug measuring cylinder

with stopper until the distillation temperature reaches to 75 oC. Heating process

is stopped at 75oC. Taking away the plug cylinder and record the distillate

volume (V1).

A.6.3 20mL of distilled water is added to the measuring cylinder where the

mixture shall be shaken up and down for 10 times (about 0.5 minute) for even

distribution. The mixture shall then be allowed to stand for 30 minutes to

become oil-water two-phase conditions. The volume of the upper layer of liquid

(oil) shall be recorded (V2).

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A.7 Calculation

Methanol content in the sample is calculated as follows:

X =𝑉1 − 𝑉2

100

Where,

X: Methanol content in the sample (volume fraction; %);

V1: Distillate from the sample before reaching 75oC (mL);

V2: The volume of the upper layer after water phase separation (mL)

A.8 Results

Repeat the experiment twice where the relative error shall be less than 0.5%.

The result shall be the average value of the experiments.

Remarks:

NOTE 1: Danger (Warning) - the sample is flammable and shall be kept away from heat

and open flame. The sample vapor is toxic, inhalation shall be carefully avoided. Containers

shall be sealed, keeping environment ventilated when used.

NOTE 2: When shaking the sample, volatile gases will be produced. Therefore the mixture

shall be uniformly mixed with a loose stopper cylinder, allowing the gas to be evaporated,

preventing pop-out.

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Appendix B (Normative):

Determination for Methanol Content of M15 Methanol Gasoline

for Motor Vehicles (Gas Chromatography)

B.1 Scope

B.1.1 This method is applicable to determine the methanol content of M15

methanol gasoline by gas chromatography.

B.1.2 This method can complete the qualitative and quantitative

determinations of methanol content, but not all components, in methanol

gasoline for motor vehicles.

B.2 Method summary

B.2.1 This method uses a packed column, hydrogen flame ionization detector.

The sample is added with standard anhydrous ethanol, and then be

quantitatively diluted with distilled water, standing for static separation.

According to internal standard method, the methanol content of M15 methanol

gasoline can be calculated by analyzing the content of methanol in aqueous

phase.

B.3 Instruments and equipment

B.3.1 Gas Chromatograph

B.3.2 Detector: Hydrogen flame ionization detector (FID)

B.3.3 Chromatography workstation

B.3.4 Column: Porapark T packed column Φ3mm × 1m

B.3.5 Micro-injector: 10μL or 5μL

B.3.6 Nitrogen: high-pressure gas bottles

B.3.7 Hydrogen: Hydrogen generator or high-pressure gas bottles

B.3.8 Air: air compressor

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B.4 Reagents and materials

B.4.1 Anhydrous ethanol (purity of 99.5%)

B.4.2 Anhydrous methanol (purity of 99.5%)

B.5 Chromatographic conditions

B.5.1 Column length: 2m

B.5.2 Column temperature: 50oC

B.5.3 Detection temperature: 200oC

B.5.4 Injection volume: 1μL

B.5.5 Detector: FID

B.5.6 Nitrogen: 30 mL / min

B.5.7 Hydrogen: 30 mL / min (carrier gas)

B.5.8 Air: 300 mL / min

B.6 Testing procedures

B.6.1 Sample preparation

The sample and the internal standard substances are extracted by 20.00mL

and 4.00mL respectively, and then diluted accurately to 100mL with distilled

water as the solvent, standing for separation. The aqueous phase separated

from the solution shall then be collected.

(NOTE: The sample, internal standard substances, solvent and any other

instruments for volume calculations, shall be used at the same temperature.)

B.6.2 Chromatography

The chromatography shall be started according to adjusted testing conditions,

until the instrument becomes stable, the water-containing solution of the

sample (which contains internal standard substances) shall be directly injected

of 1μL by a micro-injector.

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B.6.3 For determining the relative correction factor of methanol and internal

standard substances, anhydrous methanol and gasoline shall be accurately

formulated to M15 methanol gasoline of exactly 30.0% methanol content. The

sample and the internal standard substances are extracted by 20.00mL and

4.00mL respectively, and then diluted accurately to 100mL with distilled water

as the solvent, standing for separation. The aqueous phase separated from the

solution is collected by 1μL by a micro-injector for analysis. The experiment

shall be repeated for 3 times, and the average of the peak values of area ratio

of methanol to internal substances shall be the relative correction factor.

B.6.4 Typical chromatogram of sample

Fig.1. Typical chromatogram of sample

B.6.5 Depending on different equipment, selecting the best chromatographic

testing conditions through experiments. The results are most accurate when

achieving complete separation of methanol and the remaining components.