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Green Economy Initiatives Private Limited

CIN: U74900PB2013PTC038026
215 Silver City (Main)│Ambala Chandigarh Expressway (NH-22)│Zirakpur│District SAS Nagar (Mohali)
140603 Punjab│INDIA www.greenalliance.in

GEI 07-010422 F4.9-08 Handling and Analysis Instructions


PT Scheme: 22EM02P3 Ending 30.11.22

PT Item details:
Measurand (Analyte/Parameter) PT item supplied
SO2, NO2 1 x 1 Pouch marked 22EM02P3 SO2 (A) for SO2 @1gm sample
1 x 1 Pouch marked 22EM02P3 SO2 (B) for SO2 @1gm sample
1 x 1 HDPE Bottle marked 22EM02P3 NO2 for NO2 @ 8 mL sample

Instructions for Analysis- GENERAL

Suggested period of analysis: Preferably start analysis within 3 Days from date of receipt of sample
Labs can do analysis any time before last date for submission of results unless instructed otherwise in specific instructions as
stability of PT Item is examined over period of run for the scheme. However, as a good practice lab can start analysis as soon
as possible after receipt and can submit the result sheet before time to help early completion of the scheme. Please
follow specific instructions further as given in instruction sheet.

- PT item be stored on receipt from the time of arrival at laboratory


- HDPE bottle(s) with liquid sample at 2-10 °C in a refrigerator
• Pouch / Petri dish/ Vial with powdery / solid / slurry / filter paper - Keep in earmarked area at
room temperature in cool dry moisture free environment away from direct sunlight.
PRECAUTION: BEING A LABORATORY IT IS EXPECTED THAT SAMPLES ARE HANDLED BY
TRAINED AND AUTHORIZED PERSONS WHO ARE AWARE OF HANDLING AND SAFETY
ISSUES RELATED TO TEST PARAMETERS AND HAZARDOUS INVOLVED. IF ANY DOUBT
CONTACT ON GIVEN NUMBERS/ EMAIL

- PT items should be equilibrated at room temperature 25±2°C before any dilutions or analyses are
performed
- Results should be corrected for recovery and blank, if appropriate and if this is the normal practice in
the laboratory. If the sample is diluted as part of the analytical process (This is apart from the dilutions given
under specific instructions) such dilutions should be corrected for.
- The dilutions specified should be conducted in such a way as to ensure that any errors introduced by this
dilution are much smaller than the analytical errors involved in your method. As a general rule it is suggested
that the error from dilution should be less than 1%
- Samples should be treated like routine samples and all normal quality control procedures should be
adopted.

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Specific instructions for handling, analysis

Measura PT item supplied Quantity @ Specific instructions for handling, analysis


nd(s)

SO2 Sample Pouch @1gm Participants to weigh accurately 0.5 gm Powder-A and 0.15 gm
Powder-B and transfer to a clean 50 mL volumetric flask and
marked pour 15 ml of 80 percent isopropanol and 15 ml of 3 percent
22EM02P3 (A) hydrogen peroxide and dilute to the mark with reagent water*..
SO2 @1gm This is your impinger solution for analysis as per IS: 11255 P2.
NOTE: Do not correct results for this dilution
Sample Pouch
marked Start from Section 8.4 of IS: 11255 P2....Pipette a 10 ml
aliquot of impinger solution into a flask. Add 40 mL of iso-
22EM02P3 (B) propanol and two to four drops of thorin indicator. Titrate to
SO2 pink end point using 0.01 N barium perchlorate and report
volume of barium perchlorate titrant used for sample in ml.

Report your result as the titre standardized to 0.01 N barium


perchlorate e.g. a titre of 25 mL using 0.009 N barium perchlorate
equals 25 x 0.009/0.01 = 22.50 mL (resultant calculated value in
terms of 0.01 N Barium perchlorate)
NO2 HDPE Bottle 8 mL Take 1.5 ml from the solution provided by PT Provider in 50
marked mL volumetric flask and add 25 mL of absorbing solution
22EM02P3 NO2 (Section 4.1 of IS 11255 P7 2005) followed by 10 mL
reagent grade water* and NaOH sodium hydroxide (1N)
drop wise until the pH is between 9 and 12 (about 25 to 35
drops each) Dilute to mark with reagent grade water* and
mix thoroughly. NOTE: Do not correct results for this
dilution. Pipette 25 ml aliquot of the sample prepared into
the porcelain evaporating dish and proceed further from
evaporation step as in Clause 5.2 IS 11255 P7 2005. report
results of NO2 ug in 25 mL aliquot taken

Please Note
C µg NO2 in 25mL aliquote = (As-Ab) x Kc x F
Where
As= Absorbance of sample
Ab= Absorbance of blank
Kc= Spectrohotometer calibration factor
F= Dilution factor

As instructed 2= 50/25 the aliquot factor is not to be used

Further also Note that while preparing calibration curve as per


Clause 6 of IS 11255 Part-7 were with 0, 2, 4,6,8 ml KNO3
working standard solution 1ml= 100 ug but since aliquot taken is
25 ml; 2,4,6,8 ml working standard will correspond to 100, 200,
300 and 400 ug concentration rather than 200, 400, 600 and 800
ug concentration. (For further clarity labs can also refer to CPCB
LATS/80/2013-14 clause 5.2.2, relevant clause is attached)

*Reagent grade water Grade-2 or better (IS1070) or equivalent quality.


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Parameters
S.No. Measurand Units DP Test Methods Range
(Analyte/Parameter)
1 SO2 in Stack ml 1 IS: 11255 Part-2 20.0-60.0
(volume of 0.01 N
barium perchlorate titrant
used for sample in ml)

2 NO2 in Stack µg NO2 2 IS: 11255 Part-7 80.00-150.00


(Total amount of NO2 in in 25mL Note: the aliquot factor as
microgram in the aliquote given in clause 7.2 in IS
resultant 25 ml solution) method is not to be used

Test Method: Use latest methods with amendments if any / Methods based on same principle in any other standard
method may also be used.
Range: Range is given only for limited guidance e.g. for an idea whether dilution will be required or not. It is
varied to ensure that it is not used to guess the true value and sometimes may be used as a tool to avoid
collusion or may not be provided. Typographical and clerical errors are subject to correction.
Laboratories should report the results as obtained by them irrespective of range given.
Units: This indicates the units used for the assessment of data. These are the units in which participants should
report their results. For some analytes in some schemes participants may have a choice of which units to
report their results, however, the units stipulated in this scheme description are the default units to which
any results reported using allowable alternative results will be converted to.
DP: This indicates the number of decimal places to which participants should report their measurement
results. PT provider follows IS 2: Rules for rounding off numerical values- Rounding off to unit fineness
Rule I — When the figure next beyond the last figure Or place to be retained is less than 5, the figure in the last place retained
shall be left unchanged.
Rule II When the figure next beyond the last figure or place to be retained is more than 5 or is 5 followed by any figures other than
zeros, the figure in the last place retained shall be increased by 1.
Rule III — When the figure next beyond the last figure or place to be retained is 5 alone or 5 followed by zeros only, the figure
in the last place retained shall be (a) increased by 1 if it is odd and (b) left unchanged if even (zero would be regarded as an even
number for this purpose ).

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SUMMARY OF IMPORTANT INSTRUCTIONS

• Preferably suggested period of analysis: This is just to ensure all labs do analysis around same
period. Lab can do analysis anytime during the preferable suggested period of analysis except when
specific instructions are given. It does not mean it cannot be done a day earlier or extend a day later
as samples stability is examined throughout. However, as a good practice you can start analysis as
soon as possible and can submit the result sheet before time to help early completion of the
scheme
• DP: Decimal Points to which results shall be rounded of and considered for reporting.
• Preferably type your results in result sheet. After typing the results take a print put Signatures
and Organizations Stamp scan in PDF Format and email at mentioned id (Don’t email in JPG
format or by clicking pictures from mobile as these are not clear on printing) we shall not be
responsible for any illegible entries. Reports are not to be sent by post
• Check filled result sheet thoroughly before submitting. No changes for any reason are accepted.
• Participants shall use calibrated equipment’s and or certified reference material as applicable in
line with NABL 142 for testing the parameters for which participation is made irrespective of
status of accreditation. Participants shall also keep record of all calculations, graphs and other
raw data to demonstrate that testing is done by them in their lab.

PT provider does not require any of this data along with test reports but may ask for the same if
required. The said information may also be verified by regulatory authorities or accreditation
bodies during their audits. The said information is also useful in doing root cause analysis. The
failure of laboratory to provide above information any time as asked by PTP may lead to ‘Results
Not Considered’ / Cancellation of participation and decision of PTP in this regard shall be final.
LABS ARE STRONGLY ADVISED NOT TO ENGAGE IN ANY COLLUSION. COLLUSION
IS SOLE RESPONSIBILITY AND RISK OF PARTICIPATING LAB.
• Please email your result sheet at email mentioned in report sheet once only. We shall not be
responsible for reports sent on any other ids. In case you email result sheets again and again unless
asked to do so, the sheet which is sent first time will only be considered. If your result sheet is not
received dealing person will contact you.
• The participant to use a specified method or methods in accordance with the design of the proficiency
testing scheme as given above. The participants should use a different test method only with prior
permission in writing e.g. if they want to validate a method; The risk of results not being considered
orfailure in PT scheme in such a scenario lies totally with participant.
• If you are not participating in a parameter leave the results column blank
• Results reported in a semi-quantitative manner as “less than” or “more than” a value, or results
reported as zero except where it may be appropriate to report a result of zero together with qualitative
results, will be collated and listed in the PT round report as Results not Considered’ but shall not be
included in the statistical analysis including any results that are tagged i.e. any comments are given.

Please read PT Protocol

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