p. 1



### Harcro s Chemical s Inc . 520 0 Speake rRoa

d Kansa s City , K S 6610 6 Telephone : 913/621-774

7 Fax : 913/621-774

6 E-mail : OrganicsCS@Harcros.co m 

## RECEIVED OPP T CBI C 20I3JUL 2 5 AHI h 0 3 Dat e 07/23/1 3 Documen t Contro l Offic e (DCO ) (7407M ) CBI C Contro l Numbe r Offic e o f Pollutio n Contro l an d Toxic s (OPPT ) *l*t Q U.S . Environmenta l Protectio n Agenc y (EPA ) ww w 120 0 Pennsylvani a Ave . N W Washington , D.C . 2046 0 (202-564-8930 ) Attn : TSC A Sectio n 4 4 0 CF R § 799.508 7 (Docke t # EPA-HQ-OPPT-2007-0531 )

• Scanne d & Processe

d i n 

### CI S by : SHARO N RE : Physical/Chemica l Propertie s Tes t Repor t fo r CASR N 31138-65- 5 T o Who m I t Ma

y Concern : I n accordanc e wit h EPA' s fina l rule , Testin g o f Certai n Hig h Productio n Volum e Chemicals ; Secon d Grou p o f Chemicals , publishe d i n th e Federa l Registe ro n Januar y 7 , 201 1 a t 7 6 fed . Reg . 1067 , pleas e fin d enclose d th e fina l repor t fo rth e Physical/Chemica l Propertie s o n D-gluco-Heptoni c acid , monosodiu m salt , (2.xi.) - [CAS # 31138-65-5] . Thi s stud y wa s conducte d t o fulfil l th e Physical/Chemica l Propert y testin g requirement s o f testin g categor y A a s se t fort h i n Tabl e 2 o f 4 0 CF R 799.5087{j) . I f an y furthe rinformatio n i s required , pleas e d o not hesitat e t o contact m e at (913 ) 621-780 2 o rat asav i n i @harcros
. com . Regards ,

An n Mari e Savin i Harcro s Chemical s Inc . Regulator y Specialis t cc : Pete rRadford Jame s Grantha m Rand y Buckne r Joh n Mile s Fil ep . 2



## REPOR T 

# harla n

Sodiu m Glucoheptonat

e (E C 250-480-2) : Determinatio

n o f Genera l Physico-Chemica

l Propertie

s

Stud y Director : Tes tFacility :

Sponsor : RE Butle r Harla n Laboratorie s Ltd . Shardlow Busines s Par

k Shardlow Derbyshir e DE7 2 2G D U K Harcro s Chemical s Inc . 345 2 Corporat

e Driv e Dalto n G A 3072 0 US A Harla n Stud

y Number : Stud y Completion Date : 4110468 6
1 8 July 201 3

Pag e 1 o f 2 2p . 3 Harla n Stud y Number : 4110468 6 Repor

t Pag e 2 

## CONTENT S CONTENT S 2 STUD Y DIRECTO RSTATEMEN T OF GL P COMPLIANC E 3 QUALIT Y ASSURANC E STATEMENT 4 SUMMAR Y 5 GENERAL INFORMATIO N 6 Schedul e 6 Deviation s fromStud

y Pla n 6 Archivin g 6 1 INTRODUCTIO N AN D PURPOS E 7 1. 1 Guideline s /

Regulation s 7 2 TES T ITE M 8 3 METHOD S 9 3. 1 Melting/Freezin g Temperatur e 9 3.1. 1 Tes t

Syste m9 3.1. 2 Principl e o f

th e Test 9 3.1. 3 Procedur

e 9 3.1. 4 Calculatio n 9 3.1. 5 Results 1 0 3.1. 6 Conclusio n 1 0 3. 2 Boilin g Temperatur e 1 1 3.2. 1 Tes t

Syste m1 1 3.2. 2 Principl e o f

th e Test 1 1 3.2. 3 Performanc e o f

th e Tes t 1 1 3.2. 4 Dat

aHandlin g 1 2 3.2. 5 Results 1 3 3.2. 6 Discussion 1 5 3.2. 7 Conclusio n 1 5 3. 3 Wate

r Solubility 1 6 3.3. 1 Tes t

Syste m1 6 3.3. 2 Principl e o f

th e Test 1 6 3.3. 3 Performanc e o f

th e Test 1 6 3.3. 4 Results 1 8 3.3. 5 Discussio n 1 9 3.3. 6 Conclusio n 1 9 3. 4 Moisture Conten t 2 0 3.4. 1 Tes t

Syste m2 0 3.4. 2 Principl e o f

th e Test 2 0 3.4. 3 Performanc e o f

th e Tes t 2 0 3.4. 4 Calculatio n 2 0 3.4. 5 Results 2 1 3.4. 6 Discussion 2 1 3.4. 7 Conclusio n 2 1 APPENDIX 2 2 Monitorin g Authority Statemen t o f GL P Compliance 22p . 4 Harla n Stud y Number : 4110468 6 Repor

t Pag e 3 

## STUD Y DIRECTO RSTATEMEN T O F GL P COMPLIANC E Harla n Laboratorie s Ltd , Shardlow Busines s Park, Shardlow , Derbyshire , DE7 2 2GD , UK .

Thi s stud y wa s performe di n complianc e wit h U K GL P standards (Schedul

e 1 , Goo d Laborator

y Practic e Regulation s 1999 (S I 1999/3106 a s amende d b y S I 2004/0994)) . Thes e Regulation s ar

e i n accordanc

e wit h GLP standard

s published a

s OECD Principle s o n Goo d Laborator y Practice (revised1997 , ENV/MC/CHEM(98)17) ; an d ar e i n accordanc

e with , an

d implement , th

e requirements o f

Directive s 2004/9/E

C an d 2004/10/EC . Thes e principle s ar

e compatibl e wit h Good Laborator y Practic e regulation s specifie d b y regulator y authoritie s throughout

th e Europea n Community , th

e Unite dState s (EP

A an d FDA) , an dJapa n (MHLW , MAF F an

dMETI) . Thi s repor

t full y an daccuratel

y reflect s th

e procedure s use

d an d dat agenerated . Ther

e wer e n o circumstance s consideredto hav e affecte d th

e integrit y o f th e stud y o r th e validit y o f

th e data . Stud y Director : RE Butle r Harla n Stud y Number : Stud y Title : 4110468 6 Sodiu mGlucoheptonat

e (E C 250-480-2) : Determinatio n o f

Genera l Physico-Chemica

l Propertie s

Date : 

## 1 8 JU L 

## 2013p . 5



### Harla n Stud y Number : 4110468 6 Repor

t Pag e 4 

## QUALIT Y ASSURANC E STATEMEN T Harla n Stud y Number: 4110468 6 Stud y Title : Sodiu mGlucoheptonat

e (E C 250-480-2) : Determinatio

n o f Genera l Physico-Chemica

l Propertie s Th e genera l facilitie s an

d activitie s ar

e inspecte d a t leas t onc e ayea r an d th e result s ar e reporte d t o th e relevan t responsibl e perso n an dmanagement

. Study-relate

d procedure

s conducte d a t th e tes t facilit y wer e audite d an d inspected . Th

e details o f thes e audit s an d inspection

s ar e give n below .

Date s an d Type s o f

Q A Inspection s Reporte d t o th e relevan t Stud y Directo r

an d Tes t Facilit y Management Dat e o f Inspectio n Typ e o f Inspectio n Phas e Inspected Repor t Dat e 1 0 Octobe r 201 1 Genera

l Stud y Pla n Verificatio n N/ A 1 0 Octobe r 201 1 1 3 Apri l 201 2 Proces s - base d Pou

r Point 1 3 Apri l 201 2 05 Marc h 201 2 Proces s - base d Boilin g Temperatur e 05 Marc h 201 2 2 1 Marc h 201 2 Proces s - base d Wate

r Solubility 2 1 Marc h 201 2 2 1 Marc h 201 2 Stud y - base d Wate

r Conten t 2 1 Marc h 201 2 03 Apri l 201 2 Stud y - base d Los s o n Dryin g 03 Apri l 201 2 3 1 Octobe

r 201 2 Repor t Audi t N/ A 3 1 Octobe r 201 2 

### Th e complet e stud y pla n (includin

g Stud y Specifi c Supplement

) wa s verifie dfor

GL P complianc e a t repor t audit . Thi s statemen

t confirms tha

t thi s repor t reflect s th e ra w dat aan dth e procedure

s followed . Qualit y Assurance :



## 1 8 JU L 201 3p . 6



### Harla n Stud y Number : 4110468 6 Repor

t Pag e 5 

## SUMMAR

Y Th e genera l physico-chemica

l propertie s o f Sodiu mGlucoheptonat

e (E C 250-480-2

) hav e bee n determined. Th

e result s ar e summarize

dbelow : Melting/Freezing Temperature . Les s tha n -2 0 ° C ( < 25 3 K) usin g pou r poin t metho dB S 2000 : Par t 1 5 (equivalen

t t o IS O 3016) , designe

dt o b e compatibl

e wit h Metho d 10 2 o f th e OEC D Guidelines fo r

Testin g o f Chemicals , 2

7 Jul y 199 5 an d Metho d830.720 0 o f th e OPPT S Guidelines , Marc

h 1998 . Boilin g temperature . Th

e tes t ite mwa s determine

dt o partiall y boi l fro m11 7 ± 1 ° C (39 0 ± 1 K) a t 102.9 kP ab y differentia

l scannin g calorimetr

y usin g aprocedur

e designe d t o b e compatibl

e wit h Metho d10 3 o f th e OEC D Guideline

s fo r Testin g o f Chemicals , 2

7 Jul y 199 5 an dMetho d 830.722 0 o f th e OPPT S Guidelines , Augus

t 1996 . Wate r Solubility . Th

e wate r solubilit y o f th e tes t ite mwa s determine

dt o b e i n th e rang e o f 55. 8 t o 58.1 % w/

w a t 2 0 ± 0,5 ° C b

y visua l appraisa l usin g aprocedur

e base d o n th e flask method , designe dt o b e compatibl

e wit h Metho d10 5 o f th e OEC D Guidelines fo r

Testin g o f Chemicals , 2 7 Jul y 199 5 an dMetho d830.784 0 o f th e OPPT S Guidelines , Marc

h 1998 . Moistur e Content. Th

e moistur e conten t wa s determine

dt o b e 49.5 % w/

w (49 5 g/kg ) usin g a procedur e base d o n Metho dMT 1 7 o f th e CIPA C Handboo

k fo r th e Analysi s o f

Technica l an d Formulate dPesticides .p . 7



### Harla n Stud y Number : 4110468 6 Repor

t Pag e 6 

## GENERA L INFORMATIO N Schedul e Experimenta

l Startin g Date : Experimenta

l Completio

n Date : 10 Marc

h 201 2 0 4 Septembe

r 201 2 Deviation s fro m Stud y Pla n DeviationNo. l (1 8 Jul

y 2012 ) Preliminar y assessmen

t o f th e wate r conten t o f th e tes t ite musin g Kar l Fische r titratio n wa

s unsuccessful . I n error, astud y pla n amendmen

t wa s no t raise d t o amen d th e metho d o f determinatio

n t o alos s o

n dryin g procedure . Th

e moistur e conten t o f th e tes t ite mwa s determine dgravimetricall

y usin g aprocedur

e base d o n Metho dMT1 7 o f

th e CIPA C Handboo

k for th e Analysi s o f

Technica l an dFormulate

dPesticides . Archivin g Unles s instructe

dotherwis e b y th e Sponsor , al l origina

l dat aan d th e fina l repor

t wil l b e retaine d i n th e Harla n Laboratories Ltd , Shardlow , U K archive s fo r fiv e year s afte r whic h instructions wil l b e sough t a s t o furthe r retentio n o r disposal . Furthe

r retentio n o r retur n o f th e dat awil l b e chargeabl e t o th e Sponsor .p . 8



### Harla n Stud y Number : 4110468 6 Repor

t Pag e 7 

## 1 INTRODUCTIO N AN D PURPOS E Th e purpos e o f thi s stud y i s t o evaluat e th e genera l physico-chemica

l propertie s o f th e tes titem . 1. 1 Guideline s /

Regulation s Thi s stud y wa s designe d t o b e compatibl

e wit h th e procedure

s indicate db y th e following internationall

y accepte d guidelines an

drecommendations :
• OEC D Guidelines fo r

Testin g o f Chemicals . • U S EP A Offic e o f

Prevention, Pesticide

s an dToxi c Substances, Serie

s 830 : Produc

t Propertie s Tes t Guidelines . • Collaborativ

e Internationa

l Pesticide s Analytica

l Counci l (CIPAC) Metho

d M T 1 7 o f th e Handboo k fo r th e Analysi s o f

Technica l an dFormulate

dPesticides , 1995 .p . 9 Harla n Stud y Number : 4110468 6 Repor

t Pag e 8 

## 2 TES T ITE M Informatio n a

s provide db y th

e Sponsor. Identification : Description : Batch : Purity : Expir y Date : Storag e Conditions : Sodiu mGlucoheptonat

e (E C 250-480-2 ) Dar k brow n liqui d 92100010 0 99 % 0 9 Februar y 201 5 Roo mtemperatur

e i n th e dar kp . 1 0 Harla n Stud y Number : 4110468 6 Repor

t Pag e 9 

## 3 METHOD S 3. 1 Melting/Freezin g Temperatur e 3.1. 1 Tes tSyste

m Th e determinatio n wa

s carrie dou

t using the pou

r point metho d B S 2000 : Par

t 1 5 (equivalen

t t o IS O 3016) , designe

dto b e compatible wit h Metho d 10 2 o f th e OEC D Guideline s fo r

Testing o f Chemicals , 27 July 1995 an dMetho d830.720

0 o f th e OPPT S Guidelines , Marc h 1998 . 3.1. 2 Principl e o

f th e Tes t Th e pou r poin t metho dapplie s primaril y to oily , waxy o r resin-lik e tes t items , but

ma y als o b e applie dto mixture s o

r tes t items wher

e awell-define dfreezin g temperatur e i s no t observed , o

r i f agradua l but significan t

increase i n viscosit

y i s observe

d durin g cooling . 3.1. 3 Procedur

e A sampl e o f tes t ite mwa s homogenize

d b y heating a

t anomina

l temperatur

e o f 10 5 °C . Th e cooledsampl

e wa s then pouredint o ates t jar whic h wa

s then enclose

d i n aglas s jacket . Th

e sampl e wa s heate d t o 4 6 ° C i n awate

r bat h se t a t 4 8 ° C befor

e bein g allowe d to coo l i n ai r t o 3 5 °C . Th

e sampl e wa s transferre d to aice/wate r bat h maintaine d a

t - 1 ° C to 2 ° C an

d cooled t o 1 0 °C , the n transferre dt o abat

h maintaine d a

t -1 8 ° C to -1 5 ° C an

d coole d to - 7 °C , the

n finall y transferre dt

o abat h maintaine da

t -3 5 ° C t o -3 2 °C . Startin g a

t 4 6 ° C an d a t interval s o f

3 °C , th e sampl e wa s tilte dto ahorizonta

l positio n fo r

aperio do f

5 seconds , durin g whic h th e sampl e wa s observe dfo r sign s o f flow . 3.1. 4 Calculatio n Th e pou r poin t wa s calculate dusing Equatio n 3.1 . Equatio n 3. 1 P = S + 3 where : P S pou

r poin t (°C ) stationar y poin t (°C )p. 1 1 Harla n Stud y Number : 4110468 6 Repor

t Pag e 1 0

3.1. 5 Result

s Th e measure d stationar

y point s ar

e show n i n th e followin g table . Tabl e 3. 1 Measuremen

t Temperatur e (°C ) Stationar y poin t <-2 3 Pou r poin t <-2 0 3.1. 6 Conclusio n Th e pou r poin t o f th e tes t ite mha s bee n determined to b

e les s tha n -20 ° C ( < 25 3 K) .p . 1 2 Harla n Stud y Number : 4110468 6 Repor

t Pag e 1 1

3. 2 Boilin g Temperatur e 3.2. 1 Tes tSyste

m Th e determinatio n was carrie dou t b y differentia l scannin

g calorimetr

y usin g aprocedur

e designe dt o b e compatibl e wit h Metho d 10 3 o f th e OECD Guideline s fo r

Testin g o f

Chemicals , 2 7 July 199

5 an dMetho d830.722

0 o f th e OPPT S Guidelines , Augus t

1996 . 3.2.1. 1 Apparatus : Instrument : Differentia l Scannin g Calorimete

r DSC822e , Mettle

r Toled o incorporatin g ThemoHaak e Coole

r EK45/MT . Sampl e crucibles : Aluminiu mcrucibles . Lid s wit h define d perforation s wer e used . Reference crucible : Empt y aluminiu mcrucible . Test conditions : Th e test s wer e performe d i n a

n air atmosphere . 3.2.2 Principl e o

f th e Tes t A phas e transformation , e.g . meltin g o r evaporation , o

r areaction , e.g . dissociation , usually i s associate d wit h ahea

t effect . I n th

e calorimeter , tw o identical crucibles , on e fille dwit h th

e test ite man dth e othe r empt y (use da s areference) , wer

e heate d a t aconstan

t rate . Durin g th

e experiment , th

e hea t effect , i.e . th

e differenc e i n hea

t flo w betwee

n th e sampl e crucibl e an

d th e referenc e crucible , i s registered . 3.2.3 Performance o

f th e Tes t 3.2.3. 1 Calibratio n Th e temperatur

e accurac y o f th e differentia l scannin

g calorimete

r (DSC ) wa

s assesse d using a n indiu mreferenc e standar d(purity * 100%) . Th

e meltin g temperatur

e wa s determined t

o b e 156.5 3 ° C an

dwithi n the define dtoleranc e (156. 6 ± 0. 5 °C) . Th e DS C wa

s therefor e considere

d acceptabl e fo r use .

* Valu e quote

db y supplie

rp . 1 3 Harla n Stud y Number : 4110468 6 Repor

t Pag e 1 2

3.2.3. 2 Sampl

e Aliquot s (se

e followin g table ) o f

tes t ite mwer

e placed i n pre-pierce d aluminiu mcrucibles . Befor e an d after th e test , the appearanc

e o f th e samples wa

s determined . Tabl e 3.2 Determinatio

n Mas s Take n (g ) 1 0.005 4 2 0.004 9 Th e crucible s wer

e heate d u p from25 ° C t

o 45 0 °C . 3.2.4 Dat

a Handlin g Th e standar d boilin g temperatur

e i s define d a

s th e temperatur

e a t whic h the vapou

r pressur e o f a liqui di s th

e sam e a s the standar

d pressur e (101.325 kPa) . Durin g therma l analysi s th

e pea k widt h o f a n endothermic reactio n als o depend s o n sampl

e amoun t an d heatin g rate . Therefore , th e onse t poin t o f th e relevan t endothermic pea

k i s usually state

d a s th e boilin g temperature . Wher e th e endothermic peaks/effect s ar e poorl y defined , arang e wil l be state

d i n th e resul t section . Measure d temperature s wer

e converted from° C to K

using Equatio n 3.2 . Equatio n 3. 2 T = t + 273.1 5 where : T = Thermodynami c temperature , Kelvi n (K ) t = Celsiu s temperature , degree s Celsiu s (°C ) Th e boilin g temperatur

e depend s o n th e atmospheri

c pressure . A correctio n to normalize d pressur e ca n b e made , bu t

th e correctio n facto r

i s aspecifi c paramete

r fo r eac h tes t ite man d ha s to b e determined individually . A s thi s determinatio n i s beyon d the scop

e o f thi s study , n

o correctio n wil l b

e applie d t o th

e boilin g temperatur

e observed . Th

e boilin g temperatur

e i s state d wit h regar

d to th e ambien t pressur e durin g measurement .p . 1 4 Harla n Stud y Number : 4110468 6 Repor

t Pag e 1 3

3.2. 5 Result

s Thermograms an

d thermographi c dat

afo r determination s 1 an

d 2 ar e shown i n Figur

e 3. 1 an d Figur e 3. 2 an d i n th e followin g tables . Figur e 3. 1 Thermogra m -Determinatio n 1

Method: PNT81

4 170784

, 10.03.201 2 11:05:1 9

5 0 m w

Syste m 147 : METTLE R STAR ' S W 9.30

Tabl e 3.3 Thermographic Dat a - Determination 1 Therma l Even t Interpretatio n Temperatur e Therma l Even t Interpretatio n ° C K Onse t o f endother m Star t o f boiling 118.1 2 39 1 Atmospheri c pressure : 102. 9 kP aHarla n Stud y Number : 4110468 6 Repor

t p . 1 5 Pag e 1 4

Figur e 3. 2 Thermogra

m - Determination 2
Method ; PdnS M d t1.0 0 s 25.0-450.0° C 20.00°C/ml n Synchronizatio n enable

d 170764,10.03.201211:36:5 9 1707B4,4.900

0 m g

Integra l -1329.2

7 rr J Onse t 115.8 0 ° C Pea k 124.38 *

C Lef t Limi t 102.0 S " C Righ t Uml t 179.4 0 ° C RESIDUE

: dar k brow n Insid e an d outsid e o f th e crudble

4 0 6 0 8 0 10 0 12 0 14 0 16 0 18 0 20 0 22 0 24 0 26 0 28 0 30 0 32 0 34 0 36 0 38 0 40 0 42 0 ° C Hrr > J Q l i u a1

4 is is i

z I B 1 9 2 0 mi n Syste m 147 : METTLE R STAR 8 S W 9.3 0

Tabl e 3.3 Thermographi c Dat a - Determination 2 . Therma l Even t Interpretatio n Temperatur e Therma l Even t Interpretatio n ° C K Onse t o f endother m Star t o f boiling 115.8 0 38

9 Atmospheri c pressure : 102, 9 kPa Mea n boilin g temperature : Partia l boilin g from11 7 ± 1 ° C (39 0 ± 1 K )p . 1 6 Harla n Stud y Number : 4110468 6 Repor

t Pag e 1 5

3.2. 6 Discussio n Th e appearanc

e o f dar k brow n residue s bot

h insid e an d outsid e o f th e crucibl e indicate d partia l boilin g o f

th e tes t item , mos t

likel y du e to boilin g o f

th e aqueous portio n o f

th e tes t ite mleaving residue s o f

non-volatil e material . A visual determinatio n demonstrate d tha t th e test ite mstarte

d to boi l fro mapproximately 11 0 ° C whic h confirm s th

e interpretatio n o f

th e DS C thermograms . 3.2.7 Conclusio n Th e tes t ite mwa s determine dt

o partiall y boi l fro m11 7 ± 1 ° C (390 ± 1 K)a t 102. 9 kPa .p . 1 7 Harla n Stud y Number : 4110468 6 Repor

t Pag e 1 6

3. 3 Wate r Solubilit y 3.3. 1 Tes t

Syste m Th e determinatio n wa

s carrie dout

using visual appraisal , usin g aprocedur e base d o n th e flas k method , designe

dto be compatible wit h Metho d 10 5 o f th e OECD Guideline s fo r Testing o f Chemicals , 2

7 M y 1995 an

dMetho d OPPT

S 830.7840 o f

th e OPPT S Guidelines , Marc h 1998 . Th e test syste mconsistedo f

glas s double-distille dwater . 3.3.2 Principl e o

f th e Tes t To determin

e th e wate r solubility o f

th e tes t item , tw o differen t

methods ca

n b e used :

• th e colum n elutio n method , fo r

solubilitie s <10" 2g/L .

• th e flas k method , fo r

solubilitie s >10" 2g/L , o r i f th e tes t ite mi s no t

applicabl e t

o th e colum n elutio n method , e.g . liquids . 3.3.3 Performance o

f th e Tes t Th e tes t ite mwa s homogenizedb y heatin g to approximately 10

0 ° C fo r approximately 5 hour

s an dthen cooledto roo mtemperatur e prio r t o testing . 3.3.3. 1 Preliminar

y Tes t Mixture s (se

e followin g table ) o f

tes t ite man d glas s double-distille d wate r wer e adde d to nin e separat e glas s vessels . Tabl e 3. 4 Sampl e Nomina

l Concentratio

n (%w/w) Mas

s o f Tes t Ite m(g ) Mas

s o f Wate r (g) 1 1

0 1.004 4 9.095 6 2 2

0 2.054 9 8.044 7 3 3

0 3.043 4 7.074 4 4 4

0 4.047 8 6.069 3 5 5

0 5.039 5 5.010 0 6 6

0 6.018 9 4.001 9 7 7

0 7.054 9 3.017 9 8 8

0 8.048 9 2.057 5 9 9

0 9.084 9 1.059 8p . 1 8 Harla n Stud y Number : 4110468 6 Repor

t Pag e 1 7

Afte r preparation , th

e samples wer

e shake n a t approximately 3 0 ° C fo r 19! 4 hours . Afte r standing a t 2 0 ° C fo r aperio do f

2 4 hours , th

e content s o f th e vessel s wer

e visuall y appraised . Th e p H o f eac h solutio n wa

s measured . 3.3.3. 2 Definitiv e Tes t Base d o n th e result o f the preliminar

y test , mixture s (se

e followin g table ) o f

tes t ite man d glas s double-distille dwate

r wer e adde d to afurthe r

si x separat

e glas s vessels . Tabl e 3. 5 Sampl e Nomina

l Concentratio

n (%w/w) Mas

s o f Tes t Ite m(g ) Mas

s o f Wate r (g) 10 5

0 5.019 9 5.007 9 1 1 5

2 5.206 0 4.809 4 1 2 5

4 5.420 0 4.650 1 1 3 5

6 5.595 0 4.429 0 1 4 5 8 5.830 2 4.202 8 15 6

0 5.997 1 4.003 9 Afte r preparation , th

e sample s wer

e shake n a t approximatel

y 3 0 ° C fo r

7 2 hours . Afte r

standin g a t 2 0 ° C fo r aperio do f

2 4 hours , th

e content s o f th e vessel s wer

e visuall y appraised . Th e p H o f eac h solutio n wa

s measured .p . 1 9 Harla n Stud y Number

: 4110468 6 Repor

t Pag e 1 8

3.3. 4 Result

s 3.3.4. 1 Preliminar

y Tes t Th e sampl e concentrations , observation s an d solutio n pH' s ar

e shown i n the followin g table : Tabl e 3.6 Sampl e Concentratio

n ( % w/w ) Observation s Solutio n p H 1 9.9

5 Clea

r orange , homogenous, non-viscou

s solution . 9. 8 2 20. 3 Clea r dar k orange/brown

, homogenous, non-viscou

s solution . 9. 8 3 30. 1 Clea r dar k brown , homogenous, non-viscou s solution . 9.9 4 40. 0 Translucen t dar k brown , homogenous, non-viscou s solution . 9.9 5 50. 1 Opaqu e black/brown, homogenous, non-viscou s solution . 10. 0 6 60. 1 Opaqu e black/brown , homogenous, non-viscou s solutio n containin

g undissolve d tes t item . 10. 1 7 70. 0 Opaqu e black/brown , homogenous, non-viscou s solutio n containin

g undissolve d tes t item . 10. 2 8 79. 6 Opaqu e black/brown , homogenous, non-viscou s solutio n containin

g undissolve d tes t item . 10. 4 9 89. 6 Opaqu e black/brown , non-viscou

s solutio n containin

g undissolve

d tes t item . 10.

5 Result : Wate

r solubility i n th

e rang e 50. 1 to 60. 1 %w/ w a

t 2 0 ± 0. 5 °C . 3.3.4. 2 Definitiv e Tes t Th e sampl e concentrations , observation s an d solutio n pH' s ar

e show n i n th e followin g table : Tabl e 3. 7 Sampl e Concentratio

n ( % w/w ) Observation s Solutio n p H 1 0 50. 1 Opaqu e black/brown , homogenous, non-viscou s solution . 9. 7 1 1 52. 0 Opaqu e black/brown , homogenous, non-viscou s solution . 9. 7 1 2 53. 8 Opaqu e black/brown , homogenous, non-viscou s solution . 9. 7 1 3 55. 8 Opaqu e black/brown, homogenous, non-viscou s solution . 9. 7 1 4 58. 1 Opaqu e black/brown, non-viscou

s solutio n containin

g undissolve

d tes t item . 9.

7 15 60. 0 Opaqu e black/brown , non-viscou

s solutio n containin

g undissolve

d tes t item . 9.

7 Result : Wate

r solubility i n th

e rang e 55. 8 to 58. 1 %w/

w a t 2 0 ± 0. 5 °C .p . 2 0 Harla n Stud y Number : 4110468 6 Repor

t Pag e 1 9

3.3. 5 Discussio n Du e to th e hig h leve l o f

wate r solubility o f

th e tes t item , the tes t

wa s performe d b y visua

l assessment

. 3.3. 6 Conclusio n Th e wate r solubility o f

the tes t ite mwa s determined to b

e i n th e rang e o f 55. 8 to 58.1 % w/ w a

t 2 0 ±0. 5 °C .p . 2 1 Harla n Stud y Number : 4110468 6 Repor

t Pag e 2 0

3. 4 Moistur e Conten t 3.4. 1 Tes tSyste

m Th e moistur e conten t was determined b y alos s o n dryin g techniqu e base d o n procedure s outline di n Metho dM T 1 7 o f th e CIPA C Handboo

k fo r the Analysi s o f

Technica

l an d FormulatedPesticides . 3.4.2 Principl e o

f th e Tes t Th e sampl e i s heate d to constan

t weigh t i n a n ove n a t aspecifie dtemperature . 3.4.3 Performance o

f th e Tes t Th e tes t itemwa s homogenizedb y heating a t approximately 10

5 ° C an d then cooled to roo m temperatur

e prio r t o testing . Aliquot s (approximately 2 g ) o f tes t ite mwer

e weighed , i n triplicat e (A , B an d C ) into previously drie dan

dweighe dlos s bottles . Th e samples wer

e place di n avacuu

move n a t 4 0 ° C a t reduced pressur

e (approximatel

y 60 0 mbar ) an ddrie dfo r

6 days . Th

e vacuu move n temperatur

e wa s increased to 6

0 ° C an d th e tes t ite mfurthe r

drie dovernight . Th e samples wer

e transferre dto a

n ove n se t a t anomina

l temperatur

e o f 10 5 ° C an d drie d fo r

a furthe r 15 8 days . 3.4.4 Calculatio n Th e moistur e conten t was calculated using Equatio n 3.3 . Equatio n 3. 3 Moistur e Conten t (% ) = b- c xlO O b - a where :

c a b mas s o f

los s bottl e (g ) mas s o f los s bottl e an

d tes t ite m(g ) mas s o f los s bottl e an

d tes t ite mafter

dryin g (g )p . 2 2 Harla n Stud y Number : 4110468 6 Repor

t Pag e 2 1

3.4. 5 Result

s Sampl e A wa s los t prio r t o th e en d o f testing an

d s o onl y dat afro mdetermination s B an d C hav e bee n reported . Tabl e 3.8 Determinatio n A Determinatio n B a ) Mas s o f los s bottl e (g ) 19.597 5 18.050 2 b ) Mas s o f los s bottl e an d tes t ite m(g ) 21.6568 20.087 5 c ) Mas s o f los s bottl e an d tes t ite mafte r dryin g (g) 20.632 9 19.084 6 Moistur e conten t ( % w/w ) 49. 7 49. 2 Mea n moistur e conten t ( % w/w ) 49. 5 Mea n moistur e conten t (g/kg ) 49 5 3.4. 6 Discussion Th e los s o n dryin g wa

s monitore dove

r a n extende d perio dwit h multipl e time point s determined . Thes e hav e bee n summarized i n aplo t

o f los s o n dryin g versu s tim e (days) . I t wa s observe d tha t although aplatea

u an d therefor

e constan t weigh t ha d no t bee n achieved , i t

wa s considere

d tha t sufficien t dat aha d bee n obtained to repor

t afina l en d poin t after 16 5 day s o f drying . Figure 3.3 Wate rConten t S5. 0 50. 0

• j 45. 0 jf****" ^

— 40.0 JT 

### g 3 5 0 

### f J 30. 0 / 25. 0 / 20.0\£- 0 2 0 4 0 6 0 8 0 10 0 12

0 14 0 16

0 18 0 Tim e (days ) 3.4.7 Conclusio n Th e moistur e conten t o f the tes t ite mwa s determined to b

e 49.5 % w/ w (49 5 g/kg) .p . 2 3 Harla n Stud y Number : 4110468 6 Repor

t Pag e 2 2 

## APPENDIX Monitoring Authorit

y Statemen

to f GL P Complianc

e DHj Department 'ofHealth TH E DEPARTMEN T O F HEALT H O F TH E GOVERNMEN T

O F TH E UNITE D KINGDO M GOO D LABORATOR

Y PRACTIC E STATEMEN

T O F COMPLIANC E I N ACCORDANC E WIT H DIRECTIV E 2004/9/E C TES T FACILIT

Y TES T TYPE(S ) Harla n Laboratorie s Lt d Analytical/Clinica l

DAT E O F INSPECTIO N 1 0 Jul y 201 2 A n inspectio n forcomplianc e wit h th e Principle s o f Goo d Laborator y Practic e wa s carrie d ou t a t th e abov e tes t facilit y a s par t o f th e U KGoo d Laboratory Practic e Complianc e Monitorin g Programme . Thi s statemen t confirm s that , o n th e dat e o f issue , th e U KGoo d Laboratory Practic e Monitorin g Authorit y wer e satisfie d tha t th e abov e tes t facilit y wa s operatin g I n complianc e wit h th e OEC D Principle s o f Goo d Laborator y Practice . Thi s statemen t constitute s a Goo d Laborator y Practic e Instrumen t (a s define d I n th e U KGoo d Laborator

y Practic e Regulation s 1999) . Shardlo w Busines s Par k Londo n Roa d Shardlo w Derb y DE7 2 2G D Chemistr y Environmenta l Toxicit y Environmenta l Fat e Mutagenicit y Phys/Chem . Test s Toxicolog y

•2,0/n ItZDr . Andre w J . Gra

y Head , U KGL P Monitorin g Authorit y