DRAFT IN WIDE CIRCULATION

Our Ref : CHD 36/T- Doc (10049-10052)C

Date : 11 02 2016

WATER QUALITY Sectional Committee, CHD 36

ADDRESSED TO:
1)All Members of Water Quality Sectional Committee, CHD 36
2)All others interested

Dear Sir(s)

Please find enclosed the following draft Indian Standards:

i) DOC : CHD 36 (10049)C
ii) DOC : CHD 36 (10050)C
iii) DOC : CHD 36 (10051.)C
iv) DOC : CHD 36 (10052)C
METHODS OF SAMPLING AND TEST (PHYSICAL AND CHEMICAL )FOR
WATER AND WASTE WATER :PART 5 ODOUR [SECOND REVISION OF
IS 3025(PART 5)]
METHODS OF SAMPLING AND TEST (PHYSICAL AND CHEMICAL )FOR WATER
AND WASTE WATER :PART 5 ODOUR THRESHOLD [SECOND REVISION OF
IS 3025(PART 6)]
METHODS OF SAMPLING AND TEST (PHYSICAL AND CHEMICAL )FOR
AND WASTE WATER :PART 5 TASTE THRESHOLD [SECOND REVISION OF
IS 3025(PART 7)]
IS_____/ISO 8245:1999 Water quality – Guidelines for the determination of
total organic carbon (TOC) and dissolved organic carbon (DOC)

These documents are also hosted on BIS website www.bis.org.in

Kindly examine draft Indian standard and forward your views stating any difficulties which you are likely to
experience in your business or profession, if these are finally adopted as National Standard.

Last date for comment: 11 03 2016

Comments, if any, may please be made in the format as given overleaf and mailed to the undersigned at the above
address.

In case no comments are received, we would presume your approval of the documents. However, in case we receive
any comments on the document, the same shall be put up to the Sectional Committee or necessary action.

Thanking you, Yours faithfully

Encl : As above
(Dr. R K Jha)
Scientist F&H(Chemical)
 chd@bis.org.in
fax: 011 23236428

्यापकपरिचालनिसौदा
हमाअासंदभासीएचडी 36(10049-10052)सी
ददिांक: 11 02 2016

तकनीकीसमितत :पानीकी गुणव्ता,सीएचडी 36

राप्
तकताा
1 सीएचडी36कसभीसदसय
्
2 यािकाय् चअेिवानरि्

मह दय,)यय(
कृपयाािमिलनखेतमस
् दाराप्तकअं :

i) सीएचडी36 (10049)सी पािीऔअरपलि्टजनकलनएिमूि् निऔअपअीषण (भ ातकऔअअासायािक)

कीवव ि: भाग 5 गंि [IS 3025(भाग 5)का्दस
ू अापुिऱीषण]
i) सीएचडी36 (10050)सी पािीऔअरपलि्टजनकलनएिमूि् निऔअपअीषण (भ ातकऔअअासायािक)
कीवव ि: भाग6 गंिसीमा [IS 3025(भाग्6)का्दस
ू अा्पुिऱीषण]
i) सीएचडी36 (10051)सी पािीऔअरपलि्टजनकलनएिमूि् निऔअपअीषण (भ ातकऔअअासायािक)
कीवव ि: भाग 7 ्वादसीमा[IS 3025(भाग 7)का्दस
ू अापुिऱीषण]
i) सीएचडी36 (10052)सी आईएस____/आईएसओ् 8245:् 1999् पािी् की् गुणव्ता् -् कुन् जववक्
का्ाि(टीओसी) औअ् भंग् का्ाािक् का्ाि् (डीओसी)क् ाििााअण् क् लनए्
ददिाािदे ि्

ं
कृपयाइसमस दकारवन किकअं औअरपिीसम्मातय यह्तातह ु एभजककयददयहमस दाअाष्रीयमािकक्पमं रकालितह त इ
सपअरमनकअिमं आपकवयवसायरथवाकाअ
् ं
्ाअमं क्याकदििाइय आसकतीहं ।

ं जनेकीअंततिततथि11 03 2016
सि‍िततय भे

सम् ं
मातय यददक ईह त कृपयारि हस्ताअषषतक उपअलनखेतपतपअसंनग्िफ मेटमं भजं।

यददक ईसममातराप
् तिहींह तीहरथवासम्मातमं कवनभाषासं्िीरुदटहुईत उपअ क्
् तरनेक यथावतरंातम्पदददयाजाएगा
।यदद
सम्
माततकिीकीरकृातकीहुईत ववषयसलमातकरि्
यषकपअामिासरथवाउिकीइच्छापअआगकीकायावाहीकलनएववषयसलमात
क भजजािक्ादरनेक रंातम्पदददयाजाएगा।

िि्यावाद,
भवदीय
संनग्
ितलनखेतउपअ क्:
ड आअकझा
 IS _______:2016
ISO 8245: 1999
Doc No. CHD 36 (10052)C

भारतीय मानक मसौदा

पानी की गुणव्ता - कुल जववक का्बन क नन्ाबरण (टीओसी) क ललए दिशाननिे श और भंग
का्बननक का्बन (डीओसी)

Draft Indian Standard

WATRER QUALITY — GUIDELINES FOR DETERMINATION OF TOTAL ORGANIC

CARBON (TOC) AND DISSOLVED ORGANIC CARBON (DOC)

ICS 13.060,50

© BIS 2016
BUREAU OF INDIAN STANDARDS
MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG
NEW DELHI 110002

Feb 2016 Price Group

Water Quality Sectional Committee, CHD 36

NATIONAL FOREWORD

This Indian Standard which is identical withISO 8245: 1999 ‘Water quality — Guidelines for
thedetermination of total organic carbon (TOC)and dissolved organic carbon (DOC)’issued by the
International Organization for Standardization (ISO) was adopted by the Bureau of Indian Standards on
the recommendation of the Water Quality Sectional Committee and approval of the Chemical Division
Council.

The text of ISO standard has been approved as suitable for publication as an Indian Standard
without deviations. Certain conventions are, however, not identical to those used in Indian
Standards. Attention is particularly drawn to the following:

a) Wherever the words 'International Standard' appear referring to this standard, they
should be read as 'Indian Standard'

b) Comma (,) has been used as a decimal marker in the International Standard, while in
Indian Standards, the current practice is to use a point (.) as the decimal marker.

In this adopted standard, reference appears to certain International Standards for which Indian
Standards also exist. The corresponding Indian Standards, which are to be substituted in their
places, are listed below along with their degree of equivalence for editions indicated:
International Standard Corresponding Indian Standard Degree of Equivalence
ISO 5667-3:2012 Water IS 3025 (Part 1): 1987 Methods of Technically Equivalent
quality –Sampling -- Part 3: sampling and test (Physical and
Guidance on the preservation chemical) for water and wastewater:
and handling of water samples Part 1 Sampling (First Revision)

The technical committee responsible for the preparation of this standard has reviewed the provisions
of the following mentioned ISO Standards and has decided that they are acceptable for use in
conjunction with this standard:

International standard Title

ISO 5667-1 Water quality – Sampling – Part 1 : Guidance on the design of

sampling programmes
ISO 5667 - 2 Water quality – Sampling – Part 2 : Guidance on sampling
techniques
ISO 8466-1 Water quality – Calibration and evaluation of analytical methods
and estimation of performance characteristics – Part 1: Statistical
evaluation of the linear calibration function.
ISO 8466-2 Water quality – Calibration and evaluation of analytical methods
and estimation of performance characteristics – Part 2:
Calibration strategy for non-linear second order calibration
functions.
The applicable Standard atmospheric Conditions (SAC) for tropical/subtropical countries like
Indiaare 27 ± 2oC and 65 ± 5 percent relation humidity shall be observed while using this standard.

In reporting the result of a test or analysis made in accordance with this standard, is to be rounded
off, it shall be done in accordance with IS 2: 1960 ‘Rules for rounding off numerical values
(revised )’.
INTERNATIONAL ISO
STANDARD 8245

Second edition
1999-03-01

Water quality — Guidelines for the

determination of total organic carbon (TOC)
and dissolved organic carbon (DOC)
Qualité de l'eau — Lignes directrices pour le dosage du carbone organique
total (COT) et carbone organique dissous (COD)

A Reference number
ISO 8245:1999(E)
ISO 8245:1999(E)

Contents

1 Scope ........................................................................................................................................................................ 1

2 Normative reference ................................................................................................................................................ 1

3 Terms and definitions ............................................................................................................................................. 1

4 Principle.................................................................................................................................................................... 2

5 Reagents................................................................................................................................................................... 2

6 Apparatus ................................................................................................................................................................. 4

7 Sampling and samples ............................................................................................................................................ 4

7.1 Sampling................................................................................................................................................................ 4

7.2 Preparation of the water sample ......................................................................................................................... 4

8 Procedure ................................................................................................................................................................. 5

8.1 Calibration ............................................................................................................................................................. 5

8.2 Control procedures............................................................................................................................................... 5

8.3 Determination........................................................................................................................................................ 5

9 Expression of results .............................................................................................................................................. 6

9.1 Method of calculation........................................................................................................................................... 6

9.2 Precision................................................................................................................................................................ 6

10 Test report .............................................................................................................................................................. 7

Annex A (informative) Results of an interlaboratory trial for TOC determination ................................................ 8

Annex B (informative) TOC determination for samples containing particles ....................................................... 9

Bibliography .............................................................................................................................................................. 11

© ISO 1999
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic
or mechanical, including photocopying and microfilm, without permission in writing from the publisher.
International Organization for Standardization
Case postale 56 • CH-1211 Genève 20 • Switzerland
Internet iso@iso.ch
Printed in Switzerland

ii
© ISO ISO 8245:1999(E)

Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO
member bodies). The work of preparing International Standards is normally carried out through ISO technical
committees. Each member body interested in a subject for which a technical committee has been established has
the right to be represented on that committee. International organizations, governmental and non-governmental, in
liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical
Commission (IEC) on all matters of electrotechnical standardization.

International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3.

Draft International Standards adopted by the technical committees are circulated to the member bodies for voting.
Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.

International Standard ISO 8245 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee
SC 2, Physical, chemical and biochemical methods.

This second edition cancels and replaces the first edition (ISO 8245:1987) which has been technically revised.

Annexes A and B of this International Standard are for information only.

ISO 8245:1999(E) © ISO

Introduction

It is absolutely essential that tests conducted in accordance with this International Standard be carried out by suitably
qualified staff.

Total organic carbon (TOC) is a measure of the carbon content of dissolved and undissolved organic matter present in
water. It does not give information on the nature of the organic substance.

iv
INTERNATIONAL STANDARD © ISO ISO 8245:1999(E)

Water quality — Guidelines for the determination of total organic

carbon (TOC) and dissolved organic carbon (DOC)

1 Scope

This International Standard gives guidance for the determination of total carbon (TC), total inorganic carbon (TIC) and
total organic carbon (TOC) in drinking water, ground water, surface water, sea water and waste water. It also defines
terms and specifies interferences, reagents, and sample pretreatment for water samples.

The method described in this International Standard applies to water samples containing organic carbon content
ranging from 0,3 mg/l to 1000 mg/l. The lower limit concentration is only applicable in special cases, for example
drinking water, measured by highly sensitive instruments. Higher concentrations may be determined after appropriate
dilution.

This International Standard does not deal with the instrument-dependent specifications.

Purgeable organic substances, such as benzene, toluene, cyclohexane and chloroform, can also be determined using
this method.

Cyanide, cyanate and particles of elemental carbon (soot), when present in the sample, can be determined together
with the organic carbon.

2 Normative reference

The following normative document contains provisions which, through reference in this text, constitute provisions of this
International Standard. For dated references, subsequent amendments to, or revisions of, this publication do not apply.
However, parties to agreements based on this International Standard are encouraged to investigate the possibility of
applying the most recent edition of the normative document indicated below. For undated references, the latest edition
of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid
International Standards.

ISO 5667-3, Water quality — Sampling — Part 3: Guidance on the preservation and handling of samples.

3 Terms and definitions

For the purposes of this International Standard, the following terms and definitions apply.

3.1
total carbon
TC
sum of organically bound and inorganically bound carbon present in water, including elemental carbon

3.2
total inorganic carbon
TIC
sum of inorganic carbon present in water in the form of elemental carbon, total carbon dioxide, carbon monoxide,
cyanide, cyanate and thiocyanate
NOTE TOC instruments most often measure TIC as CO2 originating only from hydrogencarbonates and carbonates.

1
ISO 8245:1999(E) © ISO

3.3
total organic carbon
TOC
sum of organically bound carbon present in water, bonded to dissolved or suspended matter, including cyanate,
elemental carbon and thiocyanate

3.4
dissolved organic carbon
DOC
sum of organically bound carbon present in water originating from compounds passing through a membrane filter of
0,45 mm pore size, including cyanate and thiocyanate

3.5
volatile organic carbon
VOC
purgeable organic carbon
POC
organic carbon present in water which can be purged under the conditions of this method

3.6
non-volatile organic carbon
NVOC
non-purgeable organic carbon
NPOC
organic carbon present in water which cannot be purged under the conditions of this method

4 Principle
Organic carbon (org. C) in water is oxidized to carbon dioxide by combustion, by the addition of an appropriate oxidant,
by UV radiation or any other high-energy radiation.

The application of the ultraviolet method with only oxygen as an oxidant is restricted to low polluted waters, containing
low concentrations of TOC.
NOTE In the presence of humic material, low TOC values may be obtained when UV radiation is used.

The carbon dioxide formed by oxidation is determined either directly or after reduction, for example to methane (CH4).

The final determination of CO2 is carried out by a number of different procedures, for example infrared spectrometry,
titration (preferably in non-aqueous solution), thermal conductivity, conductimetry, coulometry, CO2-sensitive sensors
and flame ionization detection (used after reduction of CO2 to methane, among others).

In addition to organic carbon, the water sample may contain carbon dioxide or ions of carbonic acid. Prior to the TOC
determination, it is essential that this inorganic carbon be removed by purging the acidified sample with a gas which is
free from CO2 and organic compounds. Alternatively, both total carbon (TC) and total inorganic carbon (TIC) may be
determined and the organic carbon content (TOC) may be calculated by subtracting the total inorganic carbon from the
TC. This method is particularly suitable for samples in which the total inorganic carbon is less than the TOC.

Purgeable organic substances, such as benzene, toluene, cyclohexane and chloroform, may partly escape upon
stripping. In the presence of these substances, the TOC concentration is determined separately or the differential
method (TC – TIC = TOC) may be applied. By using the differential method, the value of the TOC should be higher
than the TIC, or at least of similar size.

Inorganic carbon is removed by acidification and purging or is determined separately.

5 Reagents
Use only reagents of recognized analytical grade.

In this International Standard only those chemicals and gases which are used with the majority of TOC methods are
listed. Reagents shall be used according to the manufacturer's instructions, and shall, if necessary, be pretreated.

2
© ISO ISO 8245:1999(E)

5.1 Dilution water

The TOC of the water used for dilution and for preparation of the calibration standards shall be sufficiently low to be
negligible in comparison with the lowest TOC concentration to be determined (see Table 1).

The choice of the method to pretreat water intended for dilution purposes depends on the concentration range of the
sample under investigation as shown in Table 1.

NOTE For measurements of a TOC concentration < 0,5 mg/l, it is preferable to prepare water for blanks and calibration
solutions immediately prior to analysis (see Table 1).

Table 1 — Dilution water specifications

TOC of sample Maximum acceptable Dilution water:

TOC of dilution water treatment method
mg/l mg/l

< 10 0,1* UV treatment

0,3 condensation
double distillation
10 to 100 0,5 with
KMnO4/K2Cr2O7

> 100 1 distillation

* Only for ultrapure water.

5.2 Potassium hydrogenphthalate stock solution, r (org. C) = 1 000 mg/l.

Dissolve 2,125 g of potassium hydrogenphthalate (C8H5KO4) (dried for 1 h at a temperature between 105 °C and
120 °C) in a 1 000 ml one-mark volumetric flask filled with 700 ml of water (5.1), then dilute to volume with water.

The solution is stable for about 2 months if stored in a tightly stoppered bottle in a refrigerator.

5.3 Potassium hydrogenphthalate standard solution, r (org. C) = 100 mg/l.

Pipette 100 ml of the potassium hydrogenphthalate stock solution (5.2) into a 1 000 ml one-mark volumetric flask,
and dilute to volume with water (5.1).

The solution is stable for about 1 week if stored in a tightly stoppered bottle in a refrigerator.

5.4 Standard solution for the determination of inorganic carbon, r (inorg. C) = 1 000 mg/l.

Dissolve 4,415 g of sodium carbonate (Na2CO3) [dried for 1 h at (285 ± 5)°C] in a 1 000 ml one-mark volumetric
flask in approximately 500 ml of water (5.1).

Add 3,500 g of sodium hydrogencarbonate (NaHCO3) (dried for 2 h over silica gel), and dilute to volume with water
(5.1).

This solution is stable at room temperature for about 2 weeks.

3
ISO 8245:1999(E) © ISO

5.5 Standard solution, to check the operational performance of the system.

NOTE 1 In the interlaboratory trial, copper phthalocyanine has been used for this purpose. A suitable test solution of copper
phthalocyanine, r (org. C) = 100 mg/l, may be prepared as follows:

In a 1 000 ml volumetric flask, dissolve 0,256 g of copper phthalocyanine tetrasulfonic acid (tetrasodium salt)
(C32H12CuN8O12S4Na4) in 700 ml of water, and dilute to volume with water (5.1).

The solution is stable for about 2 weeks.

WARNING — This reagent is toxic.

NOTE 2 Other stable titrimetric substances may replace reagents 5.2, 5.4 and 5.5.

5.6 Non-volatile acids, for expelling the carbon dioxide, such as phosphoric acid, c(H3PO4) = 0,5 mol/l, or if
necessary, more concentrated.

5.7 Gases, such as air, nitrogen, oxygen, free from carbon dioxide and organic impurities.

Use other gases in accordance with the instrument manufacturer's specifications.

6 Apparatus

Usual laboratory apparatus and the following.

6.1 Apparatus for the determination of organic carbon.

6.2 Homogenization device, for example a magnetic stirrer with adequate performance for the homogenization of
dispersed matter, a suitable ultrasonic apparatus or a high speed stirrer.

7 Sampling and samples

7.1 Sampling

See also ISO 5667-3.

When sampling, ensure that the samples being collected are representative (particularly in the presence of
undissolved substances), and take care not to contaminate the samples with organic substances.

Collect water samples in glass or polyethylene bottles, completely filled with the sample, and, if biological activity is
suspected, acidify to pH 2 [for example with phosphoric acid (5.6)]. In some cases, loss of volatile substances may
occur upon acidification of the sample with the loss of carbon dioxide. If volatile organic compounds are suspected,
carry out the measurement without acidification and within 8 h of sampling. Otherwise, store the sample in a
refrigerator at a temperature in the range of 2 °C to 5 °C, and analyse within 7 days. If this is not possible, the
sample can be kept at –15 °C to –20 °C for several weeks.

7.2 Preparation of the water sample

If the sample is not homogeneous and it is not possible to obtain a representative sample, even after thorough
shaking, use an appropriate apparatus (see 6.2) to homogenize the sample.

The homogeneity of the sample may be verified, for example, by separately analysing samples from the upper and
lower layers of the bottle.

If only dissolved organic substances (DOC) are to be determined, filter the sample through a membrane filter,
0,45 mm pore size, which has previously been washed with hot water to completely remove adhering organic
substances. Nevertheless, the carbon content of the filtrate shall be determined and taken into account.

4
© ISO ISO 8245:1999(E)

8 Procedure

8.1 Calibration

Comparison methods (for example, IR detection) require calibration. In the case of absolute methods, for example
acidimetry or coulometry, the calibration serves the purpose of verifying the analytical system.

Calibrate the instrument according to the manufacturer's instructions.

Establish a calibration curve by analysing potassium hydrogenphthalate standard solutions of adequate

concentrations. For example, for mass concentrations ranging from 10 mg/l to 100 mg/l, prepare a series of at least
five calibration solutions from the potassium hydrogenphthalate stock solution (5.2) as follows:

a) to prepare the calibration solutions, pipette into each of a series of 100 ml volumetric flasks for example 0 ml
(blank), 1 ml, 2 ml, 3 ml, 5 ml, and 10 ml of the potassium hydrogenphthalate stock solution (5.2), and dilute to
volume with water (5.1);

b) analyse each solution and the blank solution (from the flask without added potassium hydrogenphthalate) in
accordance with the manufacturer's instructions;

c) establish a calibration curve by plotting the mass concentrations of TOC, in milligrams of carbon per litre,
against the instrument-specific response units (I);

The reciprocal value of the slope of the resulting calibration line is the calibration factor f, in milligrams of carbon per
litre.

In order to determine the TIC value, it is necessary to establish a calibration curve by analysing calibration solutions
made from the solution described in 5.4.

In order to determine the TOC value from the difference TC – TIC, it is necessary to establish a calibration curve by
analysing calibration solutions prepared from a known mixture of the standard solutions 5.3 and 5.4.

8.2 Control procedures

Analyse the test solutions (either 5.2, 5.3, 5.4 or 5.5; see note 2 in 5.5) with each series of samples in order to verify
the accuracy of the results obtained by the method.

If the deviations found are higher than specified in within-laboratory quality criteria, investigate the following causes
of error:

 malfunction of the instrument (for example in the oxidation or detection system, leakage, faults in the
temperature or the gas control);

 change in concentration of the test solution;

 contamination of the measuring assembly.

Regularly verify the entire measuring system according to the instructions of the manufacturer and for the absence
of leaks.

These control experiments are carried out in addition to the instrumental control as specified in the operating
instructions provided by the instrument manufacturer.

8.3 Determination

Determine the TOC concentrations of the samples in accordance with the instrument manufacturer's instructions.

When TOC is determined directly, prior to analysis remove the total inorganic carbon by acidifying the sample to a
pH below 2. Carefully minimize the loss of volatile organic substances.

5
ISO 8245:1999(E) © ISO

The TOC concentration should be within the working range of the calibration. This can be achieved by diluting the
sample.

Prior to each batch of TOC determinations (for example every 10 determinations), carry out appropriate control
experiments at the intervals recommended by the manufacturer or as specified by the laboratory.

After acidification, blow a stream of pure inert gas, free from CO2 and organic impurities, through the system (for
approximately 5 min) in order to remove CO2.

9 Expression of results

9.1 Method of calculation

Depending on the type of TOC instrument used, different kinds of readings may be obtained from which the TOC or
DOC concentration of the analyzed sample is calculated. In case of discontinuous measurements, these values
may be in terms of, for example, peak heights, peak areas or volume of the titrant required. Normally, peak areas
are reported. Use peak heights only if they are proportional to the concentration.

In the case of quasi-continuous TOC or DOC measurements, the CO2 concentration generated by the combustion
of the organic matter is recorded, for example as a line on a strip chart recorder. The distance of this line from the
zero line is proportional to the TOC concentration.

Calculate the mass concentration using the calibration curve (8.1).

The mass concentration of TOC or DOC, expressed in milligrams of carbon per litre, may also be obtained from the
following equation:

I ⋅ f ⋅V
(1)
Vp

where

I is the instrument specific response;

f is the calibration factor, in milligrams of carbon per litre, evaluated according to 8.1;

V is the volume, in millilitres, of the diluted water sample;

Vp is the sample volume, in millilitres, being diluted to V.

The results shall be expressed to two or three significant figures depending on the random error (precision) of the
measurement.

EXAMPLES:

r(TOC) = 0,76 mg/l or

r(TOC) = 530 mg/l or

r(TOC) = 6,32 ¥ 103 mg/l.

9.2 Precision

Information on repeatability and reproducibility, as obtained from an interlaboratory experiment, is given in annex A.

6
© ISO ISO 8245:1999(E)

10 Test report

The test report shall contain the following information:

a) a reference to this International Standard;

b) all details necessary for a complete identification of the sample tested;

c) details concerning the storage of the laboratory samples before analysis, including the time between sampling
and analysis;

d) sample pretreatment (time for settlement, filtration);

e) the mass concentration of TOC and DOC respectively in the sample, in milligrams of carbon per litre;

f) details of any deviation from the procedure specified in this International Standard or any other circumstances
that may have influenced the result.

7
 ISO 8245:1999(E) © ISO

Annex A
(informative)

Results of an interlaboratory trial for TOC determination

Table A.1

Number of
Reproducibility Repeatability analytical
Nominal Total Number results Outliers
Sample value mean Recovery Standard Variation Standard Variation of after of
TOC TOC deviation coefficient deviation coefficient laboratories elimination results
mg/l mg/l % mg/l % mg/l % of outliers

1 2,3 2,99 129,9 0,687 23 0,19 6,3 55 259 13

2 18,5 19,2 103,9 1,23 6,4 0,38 2 56 260 9
3 120 139 115,9 12,4 8,9 2,8 2 54 236 16
4 307 13,9 4,5 3,8 1,2 54 244 20
Sample 1: Copper phthalocyanine tetrasulfonic acid, tetrasodium salt.
Sample 2: Mixture of potassium hydrogenphthalate and copper phthalocyanine tetrasulfonic acid, tetrasodium salt.
Sample 3: Mixture of potassium hydrogencarbonate, potassium hydrogenphthalate and copper phthalocyanine tetrasulfonic acid,
tetrasodium salt.
Sample 4: Industrial waste water, real sample, filtered.

NOTE 1 The reason for the recovery rate of 130 % as stated for sample 1 (sample with low TOC concentration) is possibly due to
systematic errors (non-consideration or only partial consideration of the TOC concentration of the water blank).
NOTE 2 The increased recovery rate in the case of sample 3 is possibly caused by the very high TIC concentration. In similar cases,
statements from the instrument manufacturers concerning acid volume and stripping time are often not sufficient.

8
© ISO ISO 8245:1999(E)

Annex B
(informative)

TOC determination for samples containing particles

B.1 Additional conditions

The instrumental specifications for TOC measurement should at least be suitable for measuring particle sizes of
100 µm (convention).

NOTE 1 In the interlaboratory trial (see Table B.1), samples containing particles up to 100 mm have been measured.

NOTE 2 If the TOC determination of the sample containing particles does not lead to reproducible results, even after intensive
homogenization, the sample may be filtered and the TOC of the filtrate and the residue may be determined separately.

Systems based on oxidation using UV are not suitable for the determination of microcellulose, an example of
samples containing suspended matter [see B.4, Table B.1, sample 1 b)].

B.2 Test suspension for particle processing control

This test suspension serves to verify the homogenization and recovery of incompletely dissolved sample
components (particulate matter).

To prepare this suspension, place 225 mg of cellulose, (C6H10O5)n, (particle size ranging from 20 mm to 100 mm,
carbon concentration of the suspension test sample: 100 mg/l) in a 1 000 ml volumetric flask, moist with water.
Dilute to volume with water and stir with a magnetic stirrer until the suspension is homogeneous. Ultrasonic
treatment should not be used because it reduces the particle size. The mixture is stable in the refrigerator for about
2 weeks, but it is necessary to stir each time before use.

Suspensions of equally well-suited substances may also be used as test suspensions, for example for the analysis
of paper-mill effluents.

B.3 Testing for homogenization and recovery of incompletely dissolved sample

components (particle processing control)

It is advisable that for each series of analyses of samples containing solids, the homogenization and recovery of
suspended sample components (particle processing capability of the instrument) be verified by using a test
suspension (B.2). Withdrawal of an aliquot is to be made while stirring. If an autosampler is used, samples should
be continuously stirred during analysis. The mean value from a triple measurement should be between 90 mg/l and
110 mg/l, the repeatability variation coefficient should be < 10 %.

NOTE 1 For this test, particle size is important.

NOTE 2 Optimal homogenization without particle segregation is provided, for example, by an oscillating stirrer.

B.4 Performance data

See Table B.1.

9
 ISO 8245:1999(E) © ISO

Table B.1 — Results of an interlaboratory trial for TOC determination

Number of
Reproducibility Repeatability analytical
Nominal Total Number results Outliers
Sample value mean Recovery Standard Variation Standard Variation of after of
TOC TOC deviation coefficient deviation coefficient laboratories elimination results
mg/l mg/l % mg/l % mg/l % of outliers

1a 20 16,65 83,2 7,5 45,1 2 12,0 32 149 0

1b 20 0,53 2,7 0,4 75,0 0,15 27,3 15 56 10

Sample 1 a: Cellulose microcrystals (combustion determination).

Sample 1 b: Cellulose microcrystals (UV oxidation).

10
© ISO ISO 8245:1999(E)

Bibliography

[1] DÜRR, W. and MERZ, W. Evaluation of the TOC — ISO interlaboratory trial and discussion of the results, Vom
Wasser, 55, 1980, pp. 287-294.

[2] Methods for the examination of waters and associated materials. The instrumental determination of total
organic carbon, total oxygen demand and related determinands. Her Majesty's Stationery Office, London, 1995.

[3] ISO/TR 13530, Water quality — Guide to analytical quality control for water analysis.

11
ISO 8245:1999(E) © ISO

ICS 13.060.50
Price based on 11 pages
 DOC:CHD 36 (10049)C

Draft Indian Standard

IS 3025 METHODS OF SAMPLING AND TEST (PHYSICAL AND CHEMICAL) FOR
WATER AND WASTE WATER
PART 5 ODOUR
(Second Revision)

1. Scope — Prescribes a method for the determination of true odour.

1.1 This method is applicable to all types of water and waste water.

2.Preparation of Apparatus — Thoroughly clean the required number of wide-mouth glass-

stoppered bottles of about one litre capacity. Rinse them with hydrochloric acid and render them
completely odourless by repeated washing with odour-free distilled water, which can be prepared
passing distilled water through a column of granulated activated carbon.

3. Procedure

3.1 As soon as possible after collection of sample, fill a bottle (cleaned as in 2.1) half-full of
sample, insert the stopper, shake vigorously for 2 to 3 seconds and then quickly observe the
odour. The sample taken for observation of odour shall be at room temperature.

3.2 When it is desired to record the odour at an elevated temperature, make the observation after
warming the sample in a clean stoppered bottle to about 60°C.

4. Report

4.1 Report the true odour of the sample at the mouth of the bottle as rotten egg, burnt sugar,
soapy, fishy septic, aromatic, chlorinous, alcoholic odour or any other specific odour. In case it is
not possible to specify the exact nature of odour, report as agreeable or disagreeable.

4.2 A suggested method of odour classification is shown in Appendix A.

APPENDIX A
(Clause4.2)
SUGGESTED ODOUR CLASSIFICATION
A-1.The types of odours present in waste water will widely. The type of odour shall be described
by judging the degree of sweetness, pungency, smokiness and rottenness of the odour.

A-2. If the characteristic being judged is high in intensity, rate that characteristic as ‘100’; if
medium, rate it as ‘50’; and if low, rate it as ‘0’.
Note — Intermediate ratings may be used but this practice is not recommended.

A-3. The odour class can be established by comparison with the perception levels of odour
characteristics shown in Table 1. Thus, if an odour is rated a ‘100’ in sweetness, ‘50’ in
pungency, ‘0’ in smokiness, and ‘50’ in rottenness, the odour should be described as ‘estery’ or
‘alcoholic’. Reference to the chemical types that produce these odours will guide the operator in
determining whether the odour should be reported as ‘estery’ or ‘alcoholic’.

TABLE 1 ODOURS CLASSIFIED BY CHEMICAL TYPES

(Clause A-3)
Odour Characteristics
Odour Class Chemical Example
Sweetness Pungency Smokiness Rottenness Types
(1) (2) (3) (4) (5) (6) (7)
100 50 0 to 50 50 Estery Esters, ethers, lower Lacquer solvents, most
ketones fruits, many flowers
100 50 to 100 0 to 100 50 Alcoholic Phenols and cresols, Creosote, tare, smokes,
alcohols alcohol, liquor, rose and
hydrocarbons spicy flowers, spices and
herbs
50 50 0 to 50 50 Carbonyl Aldehydes, higher Rancid fats, butter, stone
ketones fruits and nuts, violets,
grasses and vegetables
50 100 0 to 50 50 Acidic Acid anhydrides, Vinegar, perspiration,
organic acids, sulphur rancid oils, resins, body
dioxide odour garbage
100 50 to 100 50 to 100 0 to 100 Halide Qulnones, oxides and Insecticides, weed killers,
ozone, halides mustly and mouldy
nitrogen compounds odours, husks, medicinal
odour, earth, peat
50 50 100 100 Sulphury Selenium compounds, Rotting fish meat,
arsenicals, cabbage, onion, sewage
mercaptans, sulphides
100 50 50 100 Unsaturated Acetylene Paint thinners, varnish,
derivatives, kerosene turpentine,
butadlene, isoprene essential oils, cucumber
100 50 0 to 50 100 Basic Vinyl monomers, Faecal odours, manure,
amines, alkalolids, fish and shellfish, stale
ammonia flowers such as lilac, lily,
jasmine and honey-suckle
 EXPLANATORY NOTE
Odour is recognised as a quality factor affecting acceptability of drinking water and food
prepared from it, tainting of fish and other aquatic organisms, and aesthetics of recreational
waters. Most organic and some inorganic chemicals contribute taste or odour. These chemicals
may originate from municipal and industrial waste discharges, natural sources, such as
decomposition of vegetable matter or from associated microbial activity.

Odour of water, though very important, cannot be determined in absolute units. Olfactory sense,
which is the most sensitive means of detecting small concentration of odoriferous substances,
lacks precision and mathematical expression nevertheless a qualitative test is prescribed. In case
of doubt as to the intensity or character of odour, a majority opinion of several observers should
be recorded.

This method supersedes clause 6 of IS : 2488 ( Part I )-1966 ‘Methods of sampling and test for
industrial effluents, Part I’ and clause 7 of IS : 3025-1964 ‘Methods of sampling and test (
physical and chemical ) for water used in industry’.
 DOC:CHD 36 (10050)C

Draft Indian Standard

IS 3025 METHODS OF SAMPLING AND TEST ( PHYSICAL AND CHEMICAL ) FOR
WATER AND WASTE WATER
PART 6 ODOUR THRESHOLD
(Second Revision)

1. Scope —Prescribes a consistant series method for the determination of threshold odour.
Thismethod is applicable to all types of water and waste water.

2. Principle — The sample of water is diluted with odour-free water until a dilution that is of
leastdefinitely perceptible odour to each tester is found. The resulting ratio by which the sample
hasbeen diluted is called the threshold odour number (T.O.). As odour sensitivity differs with
individualsand same person may also not be consistant, a panel of not less than five persons and
preferably10 persons or more is recommended. As an absolute minimum two persons are
necessary;one to make sample dilutions and other to determine threshold odour.

3. Sample Handling and Preservation — Sample shall be collected in glass bottles with glass
ortetrafluoroethylene lined closures. Plastic containers are not reliable for odour samples and
shallnot be used. Odour tests should be completed as soon as possible after collection, In
casestorage is necessary, collect at least 1000 ml sample in a bottle filled to the top, Refrigerate,
andensure that no extraneous odours are drawn into the sample.

4. Interferences — Chlorinated waters interfere with odour measurement. In such cases

dechlorinationmay be carried out by using sodium thiosulphate in exact stoichiometric quantity.
Prepare ablank to which some amount of dechlorinating agent has been added to determine if
any odour hasbeen imparted. Such odours usually disappear upon standing if excess reagent has
not beenadded.

5. Apparatus

5.1Odour Free Glassware— Glassware cleaned before use with non-odours soap and acid
cleaningsolution followed by rinsing with odour free water.

Note — Rubber, cork and plastic stoppers should not be used.

5.2Constant Temperature Bath— A water bath capable of maintaining a temperature of 60 ±

1°C.
5.3Odour Flasks— Glass stoppered 500 ml Erlenmeyer flasks or wide mouthed 500 ml
Erlenmeyerflasks with petri dishes as cover plates.

5.4Sample Bottles— Glass bottles with glass or polytetrafluoro ethylene lined closures.

5.5Pipettes— 10.0 and 1.0 ml graduated in tenths.

5.6Graduated Cylinders — 250, 200,100,50 and 25 ml.

5.7Thermometer — 0‒110°C ( ± 1°C ).

5.8Odour—Free Wafer Generator ‒ As shown in Fig. 1.

FIG. 1 ODOUR-FREE WATER GENERATOR

6. Reagent

6.lOdour— Free Water—Odour–free dilution water prepared by filteration of tap or distilled

waterthrough a bed of activated carbon. In case tap water is used, check filtered water for
residualchlorine, unusual salt concentrations or unusual high or low pH values as these may
affect odouroussamples. Water obtained from odour-free generator should be checked daily at
the temperature atwhich tests are to be conducted ( room temperature and/or 60°C ).
7. Procedure

7.1Threshold Measurement— Use a panel of five or more persons for conducting this test.
Thetotal volume of sample and odour-free water used in each test should be 200 ml. Put the
propervolume of odour-free water into flask first and then add the sample to water. Use Table 1
fordilutions and corresponding threshold numbers.

TABLE 1 THRESHOLD ODOUR NUMBER CORRESPONDING TO VARIOUS

DILUTIONS

( Clauses 7.1, 7.2.1, 7.3 and 8.1 )

Sl No. Dilution of Sample Volume Transferred Threshold Odour

to Odour Flask* Number
(1) (2) (3) (4)
i) Original sample 200 1
100 2
50 4
25 8
12.5 16
ii) Dilution A (25 ml of original sample 50 32
diluted to 200 ml) 25 64
12.5 128
iii) Dilution B (25 ml of dilution A diluted 50 256
to 200 ml) 25 512
12.5 1024
iv) Dilution C (25 ml of dilution B diluted 50 2050
to 200 ml) 25 4100
12.5 8200
* Volume in odour flask made up to 200 ml with odour-free water.

7.2 Determine approximate range of threshold odour by adding 200, 50 and 12.5 ml of sample
toseparate 500-ml glass stoppered conical flasks containing odour-free water to make a
totalvolumeof 200 ml. Use a separate flask containing odour-free water as reference for
comparison. If test is to be conducted at 60°C, heat the dilutions and reference solution in a
constant temperature bath at 60 ± 1°C. Shake the flask containing the odour-free water, remove
the stopper and sniff thevapours. Test the sample containing the least amount of odour bearing
water in the same way.If odour is detected in this dilution prepare a more dilute sample as given
in 7.2.1. If odour is notdetected in the first dilution, repeat the above procedure using the sample
containing the next higherconcentration of the odour-bearing water and continue this process
until odour is clearly detected.

7.2.1 If the sample being tested requires more extensive dilution, prepare
intermediate,dilutionsof sample as shown in Table 1 diluted to 200 ml with odour-free water.
Use this dilution forthreshold determination. Multiply the T.O. obtained by the appropriate factor
to correct for intermediatedilution. In rare cases more than one ten fold intermediate dilution step
may be required.

7.3 Based on the results obtained in the preliminary test prepare a set of dilutions with the help
ofTable 1. Insert one or more blanks in the series in the vicinity of the expected threshold
withoutknowledge of observer.

7.4 Record the observations of each tester by indicating odour in each test flask. If odour is
notedmark plus sign ( + ) it absent, indicate by a minus sign ( – ), for example match volume of
sample diluted to 200 ml against response as given below:

Volume of sample diluted to 250 ml12.5 0 25 0 50 100 200

Response – – + – + + +

8. Calculations

8.1 The threshold odour number is the dilution ratio at which odour is just detectable. In
theexample in 7.4 the first detectable odour occurred when 25 ml sample was diluted to 200 ml.
Obtainthreshold value by dividing 200 by 25 which is 8. Alternatively read value from Table 1.

8.2 Sometimes responses are anomalous. A low concentration may be called positive and a
higherconcentration in the series may be called negative. In such cases, threshold is that point
ofdetection after which no anomalies are there, for example:
 Increasing concentration
Response – – + – + + + +
Threshold
8.3 To find the most probable average threshold from large numbers of panels use
statisticalmethods ( generally geometric mean ).

EXPLANATORY NOTE
The ultimate odour testing device is the human nose. Odour tests are performed to arriveat
qualitative descriptions and approximate quantitative measurements of odour intensity.
Themethod prescribed here for intensity measurement is the threshold odour test. This method
isapplicable to samples ranging from nearly odourless natural waters to industrial wastes
withthreshold odour numbers in thousands. There are no intrinsic difficulties with highly
odouroussamples because they are diluted proportionately before being presented to the test
observers.
 Doc: CHD 36 (10051)C

Draft Indian Standard

IS 3025 METHODS OF SAMPLING AND TEST ( PHYSICAL AND CHEMICAL ) FOR
WATER AND WASTE WATER
PART 7 TASTE THRESHOLD
( Second Revision )

1. Scope — Prescribes a method for the determination of taste threshold, for quantitative
measurement of detectable taste.

1.1 This method is applicable only to water and not to waste water.

2. Apparatus

2.1Preparation of Dilutions — System for dilution is same as that described for odour threshold
tests.

2.2 For testing, blank and each dilution is transferred to 50-ml beaker and given to observer for
testing.

3. Procedure — Prepare dilution series in the same way as in case of odour threshold testing.
Take 15 ml sample in a 50-ml beaker and pair each sample with known blank sample and present
to each panelist. Ask the panelist to hold water at 40°C in as much quantity as is comfortable for
several seconds and discharge it without swallowing. Instruct the subject to record whether a
taste or after taste is detectable in the unknown sample. Submit the samples in an increasing
order of concentration until the subject’s taste threshold has been passed.

4. Precautions

4.1 Make taste tests only samples known to be safe for ingestion.

4.2 Do not use samples that may be contaminated with bacteria, virus, parasites, or toxic
chemicals such as arsenic, dechlorinating agents or that derived from an unesthetic source.

4.3 Do not make taste tests on waste water or similar untreated effluents.

4.4 Observe all sanitary and esthetic precautions with regard to apparatus and containers
containing the sample Practice hospital-level sanitation of these items.
4.5 Make analyses in a laboratory, free from interfering background odours. If possible provide
carbon filtered air at constant temperature and humidity because without such precautions the
test measures flavor and not taste.

5. Calculations — Calculate the individual threshold and threshold of panel in the same way as
described in odour threshold tests.

EXPLANATORY NOTE
Taste, like odour is one of the chemical senses. The odour sensation is stimulated by
vapourswithout physical contact with a water sample, while taste requires contact of the taste
buds with theMate1 sample to determine its palatability. Taste is simpler than odour as there may
be only four basic taste sensations: Sour, sweet, salty and bitter, The complex sensation
experienced in the mouth during the act of tasting is a combination of taste, odour, temperature
and feel, this combination is often called flavour. Taste tests usually have to deal with this
complex combination. If a water sample contains no detectable odour and is presented at near
body temperature, the resulting sensation is predominantly true tastes.

It may not be assumed that a tasteless water is most desirable, it has become almost axiomatic
that distilled water is less pleasant to drink than certain high quality waters. Accordingly there
are two distinct purposes of taste tests. The first is to measure taste intensity by the taste
threshold test.The test results are used to assess treatment required to convert a water source into
a quality drinking water supply. The second purpose of taste testing is to evaluate the consumers
judgement of thequality of a drinking water. This test involves a panel evaluationof
undilutedsamples presented as ordinarily consumed.