ASTM E806-24 用直接进样法（气相色谱法）测定液氯中四氯化碳和氯仿含量的标准试验方法

VIP专免

乔大爷开音响 2025-03-31 9 282.64KB 8 页 16星币

Designation: E806 −24
Standard Test Method for
Carbon Tetrachloride and Chloroform in Liquid Chlorine by
Direct Injection (Gas Chromatographic Procedure)
1
This standard is issued under the ﬁxed designation E806; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope*
1.1 This test method is designed for the determination of
carbon tetrachloride (CCl
4
) and chloroform (CHCl
3
) in liquid
chlorine. Carbon tetrachloride can be analyzed over a range
with an upper limit of 149 mg ⁄kg by this method. Chloroform
can also be analyzed over a range with an upper limit of
122 mg ⁄kg but may, with carbon tetrachloride, be applicable to
a wider range. The lower limit of detection is dependent on the
sample size and the instrument used. For CCl
4
the LOD is 2.4
and LOQ is 8. For CHCl
3
the LOD is 3.3 and LOQ is 11.
NOTE 1—The LOD and LOQ were calculated based on Table 1 data.
1.2 In determining the conformance of the test results using
this method to applicable speciﬁcations, results shall be
rounded off in accordance with the rounding-off method of
Practice E29.
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this
standard.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
Speciﬁc hazards statements are given in Section 7and in 9.2.3.
1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
2
D6809 Guide for Quality Control and Quality Assurance
Procedures for Aromatic Hydrocarbons and Related Ma-
terials
E29 Practice for Using Signiﬁcant Digits in Test Data to
Determine Conformance with Speciﬁcations
E180 Practice for Determining the Precision of ASTM
Methods for Analysis and Testing of Industrial and Spe-
cialty Chemicals (Withdrawn 2009)
3
E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
E806 Test Method for Carbon Tetrachloride and Chloroform
in Liquid Chlorine by Direct Injection (Gas Chromato-
graphic Procedure)
2.2 Federal Standard:
4
OSHA Regulations, 29 CFR paragraphs 19100.1000 and
1910.1200 Air Contaminates – Table of Exposure Limits
and Hazard Communication
49 CFR 173 Code of Federal Regulations Title 49 Transpor-
tation; Shippers’ General Requirements for Shipments and
Packagings, including Sections:
49 CFR 173, Section 173.304 Charging of Cylinders with
Liqueﬁed Compressed Gas
49 CFR 173, Section 173.314 Requirements for Compressed
Gases in Tank Cars
49 CFR 173, Section 173.315 Compressed Gases in Cargo
Tanks and Portable Tank Containers
1
This test method is under the jurisdiction of ASTM Committee D16 on
Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsi-
bility of Subcommittee D16.13 on Chlorine.
Current edition approved Oct. 1, 2024. Published January 2025. Originally
approved in 1981. Last previous edition approved in 2021 as E806 – 21. DOI:
10.1520/E0806-24.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at www.astm.org/contact. For Annual Book of
ASTM Standards volume information, refer to the standard’s Document Summary
page on the ASTM website.
3
The last approved version of this historical standard is referenced on
www.astm.org.
4
Available from U.S. Government Printing Office, Superintendent of
Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http://
www.access.gpo.gov.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
1

2.3 Other Document:

Chlorine Institute Pamphlet No. 1 Chlorine Basics

3. Summary of Test Method

3.1 A sample of liquid chlorine is injected into a gas

chromatograph (GC), equipped with a column capable of

separating CCl

and CHCl

from Cl

and other impurities,

using a suitable syringe. The amounts of CCl

and CHCl

the sample are determined by comparison of the areas of the

peaks, obtained with the samples, to areas of peaks obtained

with suitable calibration standards, under the same conditions.

4. Signiﬁcance and Use

4.1 CCl

and CHCl

may be present in trace amounts in

liquid chlorine. The use of chlorine to purify water would then

transfer these compounds to the water. Therefore, when the

concentrations of the CCl

and CHCl

in the liquid chlorine are

known, the maximum amounts contributed to the water by the

chlorine can be estimated.

5. Apparatus

5.1 Gas Chromatograph, equipped with:

5.1.1 Injection Port, must be lined with glass, Monel,

nickel; or column must be installed for on-column injection.

5.1.2 Septa, from Viton.

Silicone septa may produce arti-

facts that may interfere with the analysis.

5.1.3 Column, Column Materials, and Packing, must be

compatible with chlorine. Silanized supports and silanized

glass wool must be avoided. Column must be able to separate

, CCl

, and CHCl

. Columns that have been found to be

suitable are:

5.1.3.1 Nickel Tubing, 3.05 m by 3.175 mm outside

diameter, packed with 10 % sodium chloride solution on

Porasil C

(see Appendix X1 for packing preparation). This is

the preferred packing.

5.1.3.2 Polytetraﬂuoroethylene Tubing, 3.05 m by 2 mm

inside diameter, packed with 20 % Kel-F

No. 10 oil on 60/80

mesh Chromosorb

W AW.

5.1.3.3 Glass Tubing, 3.05 m by 2 mm inside diameter,

packed with 20 % Halocarbon

1025 on 60/80 mesh Chromo-

sorb W AW.

5.1.4 Flame Ionization Detector.

5.1.5 Recorder, compatible with the GC detector output.

5.1.6 Electronic Integrator (optional), compatible with the

GC detector output.

5.2 Balance, capacity 5000 g, reading to 61 g.

5.3 Autoinjectors are required for all gas chromatograph

standards using an external standard to calculate results.

6. Reagents and Materials

6.1 Purity of Reagents—Unless otherwise indicated, it is

intended that all reagents shall conform to the speciﬁcations of

the Committee on Analytical Reagents of the American Chemi-

cal Society, where such speciﬁcations are available.

Other

grades may be used, provided it is ﬁrst ascertained that the

reagent is of sufficiently high purity to permit its use without

lessening the accuracy of the determination.

6.2 Chlorine, (CAS 7782-50-5), liquid, with less than

10 µg ⁄g each of CCl

and CHCl

. This may be prepared by

condensing the gaseous phase above regular production chlo-

rine.

6.3 Carbon Tetrachloride, (CAS 56-23-5), reagent grade.

6.4 Chloroform, (CAS 56-23-5), reagent grade.

6.5 Sample Cylinder Assembly (Fig. 1), consisting of:

6.5.1 Sample Cylinders;

nickel, Monel, or tantalum (Note

2), 400 mL capacity, double-ended, specially cleaned (Note 3).

6.5.2 Valves, having a packing resistant to liquid chlorine.

6.5.3 Holder for a Septum, that can be easily assembled.

Available from The Chlorine Institute Inc., 1300 Wilson Blvd., Suite 525,

Arlington, VA 22209, https://www.chlorineinstitute.org.

Monel is a registered trademark of Special Metals Corporation.

Viton is a registered trademark of The Chemours Company.

Porasil is a trademark of Waters Associates, Inc.

Kel-F is a registered trademark of 3M Company.

Chromosorb is a registered trademark of Imerys Minerals California, Inc.

Halocarbon is a registered trademark of Halocarbon Products Corporation.

A 400 mL nickel cylinder ﬁlled with liquid chlorine weighs about 4000 g.

ACS Reagent Chemicals, Speciﬁcations and Procedures for Reagents and

Standard-Grade Reference Materials, American Chemical Society, Washington,

DC. For suggestions on the testing of reagents not listed by the American Chemical

Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,

U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-

copeial Convention, Inc. (USPC), Rockville, MD.

This reagent is used for calibration purposes only.

If samples are to be shipped outside any plant, cylinders approved by the U.S.

Department of Transportation must be used.

Packing made from Teﬂon, registered trademark of The Chemours Company,

Viton, Kel-F, or equivalent have been found suitable for this purpose.

Swagelok, registered trademark of Swagelok Company, or equivalent ﬁttings

have been found suitable for this purpose.

TABLE 1 Precision Values

Repeatability Laboratory Precision Reproducibility

Level, mg/kg

Standard

Deviation,

mg/kg

Degrees of

Freedom

95 % Limit,

mg/kg

Standard

Deviation,

mg/kg

Degrees of

Freedom

95 % Limit,

mg/kg

Standard

Deviation,

mg/kg

Degrees of

Freedom

95 % Limit,

mg/kg

Carbon Tetrachloride (CCl

)

9 0.8 44 2 1.9 11 5 5.3 10 15

62 3.9 40 11 4.6 10 13 10.4 9 29

149 6.8 44 19 7.7 11 21 21.4 10 60

Chloroform (CHCl

)

10 1.1 44 3 0.94 11 3 2.7 10 8

48 2.4 44 7 1.5 11 4 8.1 10 23

122 7.1 48 20 4.5 12 13 13.3 11 37

E806 − 24

NOTE 2—Carbon or stainless steel cylinders and ﬁttings are not suitable

as CHCl

is unstable in the presence of FeCl

and Cl

NOTE 3—A procedure for cleaning cylinders and valves, for use with

liquid chlorine, is given in Appendix X2.

6.6 Fittings, for transferring chlorine from one cylinder to

another.

6.7 Syringe, 10 µL to 100 µL, capable of holding liquid

chlorine under pressure, with 26-gauge disposable needle.

NOTE 4—Disposable needles are recommended because corrosion with

permanent needles may cause problems.

7. Hazards and Safety Precautions

7.1 Consult the current supplier Safety Data Sheet (SDS),

local and OSHA regulations concerning all materials used in

this test method such as detailed information concerning

toxicity, ﬁrst aid procedures, and safety precautions. Handle all

reagents as recommended by the supplier.

7.2 Chlorine is a corrosive, extremely dangerous, and toxic

material. A well-ventilated fume hood should be used to house

all test equipment, except the gas chromatograph which is

vented to a hood, when this product is analyzed in the

laboratory. User should refer to literature for safe handling.

Chlorine is heavy. If it gets in the lungs it is going to be difficult

to get out. In the event chlorine is inhaled, ﬁrst aid should be

summoned immediately and oxygen administered without

delay. Quick medical attention is needed before the lungs start

to dissolve as chlorine reacts with the moisture in the lungs.

7.3 Liquid chlorine sampling and analysis should be at-

tempted only by persons who are thoroughly familiar with the

handling of chlorine, and even an experienced person should

not work alone. A second person must be present. The operator

must be provided with adequate eye protection and a full face

respirator. Splashes of liquid chlorine destroy clothing and, if

such clothing is next to the skin, will produce irritations and

burns.

7.4 If liquid samples are to be taken in cylinders, do not

allow the sample cylinder to become liquid full. Test Method

E806, 49 CFR 173.314, 173.315, and 173.304 advise that the

weight of the chlorine in the cylinder should not be more than

125 % of the weight of the water that the cylinder could

contain.

7.5 Indoor sampling from a small container should be done

in a fume hood. Vent test equipment such as GCs to hoods.

Have separate Lab areas to analyze liquid chlorine to minimize

exposure risk. Personnel chlorine monitors are worn to monitor

personnel exposure.

7.6 It is recommended that means be available for disposal

of excess chlorine in an environmentally safe and acceptable

manner. If chlorine cannot be disposed of in a chlorine

consuming process, a chlorine absorption system should be

provided such as discharging the chlorine into a caustic

scrubber containing an appropriate amount of 20 % caustic

solution to neutralize all the chlorine. This reaction is

exothermic, and care should be taken to avoid excess heating

by choosing a sufficiently large volume of caustic solution to

serve as a heat sink. Chlorine does not readily disperse and will

hug the ground. Chlorine must all be adsorbed. Purging to the

atmosphere is not acceptable. When the analysis and sampling

regimen requires an initial purging of chlorine from a

container, the purged chlorine should be similarly handled.

7.7 Store pressurized samples where involuntary release

would not cause excessive risk to people or property.

8. Sampling and Handling

8.1 Sampling from tank cars, barges, storage tanks, and

large cylinders presents unique problems. Each facility,

however, must be capable of delivering a liquid sample (not

gas) for test. See Chlorine Institute Pamphlet No. 1 “Chlorine

Basics” for additional technical information regarding liquid

chlorine.

8.2 In general, no chlorine should be released to the

atmosphere. When sampling and working with chlorine out of

doors, the area should be well-ventilated and people downwind

from such operations should be warned of the possible release

FIG. 1 Sample Cylinder Assembly

E806 − 24

文档加载中……请稍候！
如果长时间未打开，您也可以点击刷新试试。

下载文档到电脑，查找使用更方便

亲，本站95%以上的标准规范都面向会员免费，办理VIP会员下载更省钱，平均每篇不到2元

立即下载 VIP免费下载

标签： #标准试验 #试验方法 #标准试验方法

摘要：

本页面详细介绍 ASTM E806-24 标准，即采用直接进样气相色谱法测定液氯中四氯化碳和氯仿含量的标准试验方法。该标准适用于工业液氯中微量杂质（四氯化碳和氯仿）的精确测定，是氯碱行业、化工品控及环境安全检测领域的核心技术规范。通过直接进样无需复杂前处理，利用气相色谱的分离能力一次性完成两种组分的定量分析，有效提升了检测效率与数据可靠性。无论是实验室研发、质量检验还是进出口贸易，遵循 ASTM E806-24 均可确保结果的一致性与国际通用性。页面旨在帮助用户快速掌握该方法的核心步骤、设备要求

展开>> 收起<<

ASTM E806-24 用直接进样法（气相色谱法）测定液氯中四氯化碳和氯仿含量的标准试验方法.pdf

共8页,预览3页

还剩页未读，继续阅读

声明：本文档系会员上传，若文档所含内容侵犯了您的版权或隐私，请立即通知，我们立即给予侵权申诉删除！

ASTM E806-24 用直接进样法（气相色谱法）测定液氯中四氯化碳和氯仿含量的标准试验方法

相关推荐

开通VIP享超值会员特权

相关内容

热门标签

举报选择: