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煤中全水分的测定方法
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GBT 211-2017
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标准编号: GB/T 211-2017 (GB/T211-2017)
中文名称: 煤中全水分的测定方法
英文名称: Determination of total moisture in coal
行业: 国家标准 (推荐)
中标分类: D21
国际标准分类: 73.040
字数估计: 10,159
发布日期: 2017-09-07
实施日期: 2018-04-01
旧标准 (被替代): GB/T 211-2007
起草单位: 煤炭科学技术研究院有限公司检测分院
归口单位: 全国煤炭标准化技术委员会(SAC/TC 42)
提出机构: 中国煤炭工业协会
发布机构: 中华人民共和国国家质量监督检验检疫总局、中国国家标准化管理委员会
GB/T 211-2017: 煤中全水分的测定方法
GB/T 211-2017 英文名称: Determination of total moisture in coal
ICS 73.040
D21
中华人民共和国国家标准
代替GB/T 211-2007
2017-09-07发布
2018-04-01实施
中华人民共和国国家质量监督检验检疫总局
中国国家标准化管理委员会发布
前言
本标准按照GB/T 1.1-2009给出的规则起草。
本标准代替GB/T 211-2007《煤中全水分的测定方法》。本标准与GB/T 211-2007相比,除编辑
性修改外,主要技术内容变化如下:
---删除了测定方法中方法C(微波干燥法)(见2007年版的3.3);
---方法B1中增加了13mm试样(见3.2.1,2007年版的3.2.1);
---增加了制样过程空气干燥的水分损失补正(见7.4);
---增加了资料性附录微波干燥法测定煤中全水分(见附录A)。
本标准使用重新起草法参考ISO 589:2008《硬煤 全水分测定》编制。与ISO 589:2008的一致性
程度为非等效。
本标准由中国煤炭工业协会提出。
本标准由全国煤炭标准化技术委员会(SAC/TC42)归口。
本标准起草单位:煤炭科学技术研究院有限公司检测分院。
本标准主要起草人:张博、孙刚、李宏图。
本标准所代替标准的历次版本的发布情况为:
---GB 211-1963、GB 211-1984、GB/T 211-1996、GB/T 211-2007。
煤中全水分的测定方法
1 范围
本标准规定了测定煤中全水分的方法提要、试剂和材料、仪器设备、样品、测定步骤、结果计算、方法
精密度和试验报告。
本标准规定的氮气干燥法(方法A1和方法B1)适用于所有煤种;空气干燥法(方法A2和方法B2)
适用于烟煤(易氧化的煤除外)和无烟煤。
本标准以方法A1作为仲裁方法。
注:本标准还给出了用于全水分快速测定的微波干燥法,微波干燥法适用于烟煤和褐煤,参见附录A。
2 规范性引用文件
下列文件对于本文件的应用是必不可少的。凡是注日期的引用文件,仅注日期的版本适用于本文
件。凡是不注日期的引用文件,其最新版本(包括所有的修改单)适用于本文件。
GB/T 212 煤的工业分析方法
GB/T 474 煤样的制备方法
GB/T 19494.2 煤炭机械化采样 第2部分:煤样的制备
3 方法提要
3.1 方法A(两步法)
3.1.1 方法A1:氮气干燥
称取一定量的13mm试样,在温度不高于40℃的环境下干燥到质量恒定,再将干燥后的试样破碎
到标称最大粒度3mm,于105℃~110℃下,在氮气流中干燥到质量恒定。根据试样经两步干燥后的
质量损失计算出全水分。
4 试剂和材料
4.1 无水氯化钙:化学纯,粒状。
4.2 变色硅胶:工业品。
4.3 氮气:纯度≥99.9%,含氧量< 0.01%。
4.4 浅盘:由搪瓷、不锈钢、镀锌铁板或铝板等耐热、耐腐蚀材料制成,其规格应能容纳500g试样,且
单位面积负荷不超过1g/cm2。
4.5 玻璃称量瓶:直径70mm,高35mm~40mm,并带有严密的磨口盖。
4.6 取样器具:适用于13mm或6mm试样,开口尺寸至少为相应粒度的3倍。
5 仪器设备
5.1 空气干燥箱:带有自动控温和鼓风装置,能控制温度在30℃~40℃和105℃~110℃范围内,有
气体进、出口,有足够的换气量,每小时可换气5次以上。
5.2 通氮干燥箱:带自动控温装置,能保持温度在105℃~110℃范围内,可容纳适量的称量瓶,且具
有较小的自由空间,有氮气进、出口,每小时可换气15次以上。
5.3 分析天平:分度值0.001g。
5.4 工业天平:分度值0.1g。
5.5 干燥器:内装变色硅胶或粒状无水氯化钙。
5.6 流量计:量程100mL/min~1000mL/min。
5.7 干燥塔:容量250mL,内装变色硅胶或粒状无水氯化钙。
7 测定步骤
7.1 方法A(两步法)
7.1.1 外在水分(方法A1和A2,空气干燥)
在预先干燥和已称量过的浅盘内迅速称取13mm的试样490g~510g(称准至0.1g),平摊在浅盘
中,于环境温度或不高于40℃的空气干燥箱中干燥到质量恒定(连续干燥1h,质量变化不超过0.5g),
记录恒定后的质量(称准至0.1g)。对于使用空气干燥箱干燥的情况,称量前需使试样在试验室环境中
重新达到湿度平衡。
7.2.3 结果计算
按式(4)计算煤中全水分:
7.3 试样水分损失补正
需要进行水分补正时,则按式(5)求出补正后的全水分值。
7.4 制样过程空气干燥的水分损失补正
如在制备全水分试样前,对煤样进行了空气干燥,造成煤样质量损失,则按式(6)求出补正后的全水
分值。
8 方法的精密度
全水分测定结果的重复性限应符合表1的规定。
试验报告应至少包括以下信息:
---试样编号;
---依据标准;
---使用的方法;
---试验结果;
---与标准的任何偏离;
---试验中出现的异常现象;
---试验日期。
GB/T 211-2017
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 73.040
D 21
Replacing GB/T 211-2007
Determination of Total Moisture in Coal
(ISO 589.2008, Hard Coal-Determination of Total Moisture, NEQ)
ISSUED ON. SEPTEMBER 7, 2017
IMPLEMENTED ON. APRIL 1, 2018
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.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative References ... 4
3 Method Summary ... 4
4 Reagent and Materials ... 5
5 Apparatus ... 5
6 Sample ... 6
7 Procedures ... 6
8 Precision of the Methods ... 10
9 Test Report ... 10
Appendix A (Informative) Determination of Total Moisture in Coal by Drying by
Microwave ... 12
Foreword
This Standard is drafted in accordance with GB/T 1.1-2009.
This Standard replaces GB/T 211-2007 “Hard Coal - Determination of Total Moisture”.
In comparison with GB/T 211-2007, in addition to editorial changes, the main technical
content changes are as follows.
— Method C (drying by microwave) is deleted (please refer to 3.3 in Version 2007);
— 13mm sample is added to Method B1 (please refer to 3.2.1 in Version 2007);
— Moisture loss correction of dry air during the sampling is added (please refer to
7.4);
— Informative appendix (determination of total moisture in coal through the method
of drying by microwave) is added (please refer to Appendix A).
This Standard is redrafted in accordance with ISO 589.2008 “Hard Coal -
Determination of Total Moisture”. The consistent degree between this Standard and
ISO 589.2008 is not equivalent.
This Standard was proposed by the China National Coal Association.
This Standard shall be under the jurisdiction of the National Technical Committee on
Coal Chemical Industry of Standardization Administration of China.
Drafting organization of this Standard. Coal Analysis and Test Laboratory of China
Coal Research Institute.
Chief drafting staffs of this Standard. Zhang Bo, Sun Gang and Li Hongtu.
The previous editions of the standard replaced by this Standard are as follows.
— GB 211-1963, GB 211-1984, GB/T 211-1996 and GB/T 211-2007.
Determination of Total Moisture in Coal
1 Scope
This Standard specifies the method summary, reagent and materials, apparatus,
procedures, result calculation, precision and test report for the determination of total
moisture in coal.
The method of drying under nitrogen (Method A1 and B1) shall be applicable to all
types of coals; the method of drying in air (Method A2 and B2) shall be applicable to
bitumite (excluding easily oxidized coal) and blind coal.
Method A1 shall be the arbitration method in this Standard.
Note. the method of drying by microwave that’s applicable to the rapid determination
of total moisture is also provided in this Standard. The method of drying by microwave
is applicable to bitumite and lignite. Please see Appendix A for details.
2 Normative References
The following documents are indispensable in the implementation of this Standard.
For the dated references, only the dated versions are applicable to this Standard. For
the undated references, the latest edition (including all the amendments) are
applicable to this Standard.
GB/T 212 “Proximate Analysis of Coal”
GB 474 “Method for Preparation of Coal Sample”
GB/T 19494.2 “Mechanical Sampling of Coal - Part 2. Method for Sample
3 Method Summary
3.1 Method A (two-stage method)
3.1.1 Method A1. drying under nitrogen
Weigh-take a certain amount of 13mm coal samples; dry them in the environment
where the temperatures do not exceed 40°C, until the constant mass is reached.
Crush the sample into particle size lower than 3mm; dry them under nitrogen at
(105~110) °C, until the constant mass is reached. Calculate the total moisture from
with a sufficiently rapid rate of atmosphere change, for instance, more than 5 times
per hour.
being controlled at (105~110)°C, able to accommodate appropriate weighing bottles
with a little more room to spare, with inlet and outlet for nitrogen, and allow more than
15 times of atmosphere change per hour.
5.3 Analytical balance. division value is 0.001g.
5.4 Industrial balance. division value is 0.1g.
5.5 Dryer. contain allochronic silica gel or granular anhydrous calcium chloride.
5.6 Flow meter. with a measuring range of (100~1000)mL/min.
5.7 Drying tower. with a volume of 250ml and contain allochronic silica gel or granular
anhydrous calcium chloride.
6.1 According to GB 474 or GB/T 19494.2, prepare the sample for total moisture. In
which, for 13mm coal sample for total moisture, it shall not be less than 3kg; for 6mm
sample for total moisture, it shall not be less than 1.25kg.
6.2 Before determining the total moisture in coal sample, it shall firstly check the
sealing condition of the container. Afterwards, clean the surface; weigh the sample
with an industrial balance to the nearest 0.1% of its total mass; check the result with
the total mass indicated on the label. If there’s a loss of mass and it can be
ascertained that there is no sample loss during transportation or storage, then the
mass reduced shall be regarded as that of the lost moisture. Calculate the percentage
the loss of mass is greater than 1.0%, then, it is not allowed to perform correction of
moisture loss; when reporting the results, it shall indicate that “the moisture loss is not
corrected” AND report the container label and sealing condition.
6.3 Before weighing-taking the sample, it shall well mix (mixing time is not less than 1
min) the sample.
7 Procedures
7.1 Method A (two-stage method)
7.1.1 Free moisture (Methods A1 and A2, drying in air)
Use a pre-dried and weighed tray to quickly take-weigh 490g~510g (accurate to 0.1g)
case, the mass of the previous inspection shall be adopted as the reference for
calculation.
7.2.2 Method B2 (drying in air)
7.2.2.1 Total moisture in 13 mm coal sample
7.2.2.1.1 Use a pre-dried and weighed tray to quickly weigh-take 490g~510g
(accurate to 0.1g) of 13 mm coal sample; spread it evenly.
7.2.2.1.2 Put the tray in an air-drying oven which has been preheated to
(105~110)°C. Under the condition of air-blowing, for bitumite, dry for 2h; for blind coal,
dry for 3h.
7.2.2.1.4 Conduct drying inspection, 30min each time, until each mass reduction in
two continuous inspections is less than 0.5g or the mass increases. In the latter case,
the mass of the previous inspection shall be adopted as the reference for calculation.
7.2.2.2 Total moisture of 6mm coal sample
Except that the nitrogen-flushed oven is replaced by the air-drying oven, the
procedures are the same as that in 7.2.1.
7.2.3 Result calculation
Total moisture in coal shall be calculated in accordance with Formula (4);
Where,
m — the mass of weighed coal sample, unit is gram (g);
m1 — the mass loss after the coal sample is dried, unit is gram (g).
7.3 Moisture loss correction in the sample
If there is a need for moisture correction, the value of corrected total moisture shall be
calculated in accordance with Formula (5).
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