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The UN said Syrian authorities had detained 336 men who left Homs and were still questioning most of them without direct supervision by any neutral third party.
The Syrian government and the opposition met face-to-face on Tuesday and observed a minute of silence for people killed in the three year conflict after a first round of talks last month failed to make significant progress, delegates said.
"I hope that the minute of silence will signal an improvement in the atmosphere this time," opposition delegate Ahmed Jakal told Reuters.
He said that international mediator Lakhdar Brahimi proposed that the two sides discuss ending the violence on Tuesday and the formation of a transitional governing body on Wednesday.
The two issues have caused deep rifts between the two sides and delayed negotiations.
Monzer Akbik, a spokesman for the opposition National Coalition, said that Tuesday's session was still focused on discussing what the schedule for the week should be and said the two sides were arguing over the length and number of meeting.
Men leaving besieged Homs detained, questioned
Syrian authorities have detained 336 men who left Homs and are still questioning most of them without direct supervision by any neutral third party, the United Nations said on Tuesday.
The men, deemed to be of fighting age by the Syrian authorities, were among 1,151 who left the besieged rebel-held Old City of Homs during an agreed ceasefire that was extended for another three days, until Wednesday.
The UN-brokered "humanitarian pause" between 6 a.m. and 6 p.m. has also allowed aid to get into the old quarter of Homs, which has been surrounded by President Bashar al-Assad's forces for more than a year and a half.
Homs governor Talal al-Barazi said around 100 men had been questioned and released, but the United Nations has so far only reported the release of 41 men.
The men have been questioned in a school, under the "general monitoring" of protection staff from the UN refugee agency UNHCR and the UN children's agency, UNHCR spokeswoman Melissa Fleming told a briefing in Geneva.
"We know every person that is there. We are speaking to them separately ... But these are interviews that the UN is not necessarily privy to. These are security screening interviews," Fleming said.
"Mostly what we're asking about is we're concerned in general about how they're faring, what's their health situation, what are their concerns," she said.
The UN was also asking detainees about the humanitarian situation inside Old Homs, she said, to better inform aid workers going back in for evacuations and aid distributions.
Aid and evacuations operations were halted on Tuesday afternoon for logistical reasons, the governor said, but will continue again on Wednesday morning at 9:30 a.m.
Most dangerous chemical weapons out by March
Meanwhile, Syria's ambassador to Russia said the most dangerous elements of President Bashar al-Assad's chemical weapons stockpile would be out of Syria by March 1, according to Interfax news agency.
Syria missed a December 31 deadline to remove its most poisonous chemical agents under a deal brokered by Russia and the United States to avert a threatened US-led military strike against Assad's forces after a chemical weapons attack last year.
Damascus also failed to give up its entire stockpile by Feb. 5, sparking worries that it would then miss a final deadline of June 30 to eliminate its chemical weapons program completely.
"A large part of the chemical weapons, the most dangerous stocks, will be taken out of the country by March 1," Interfax quoted Syrian ambassador Riad Haddad as saying. "I think we'll stick to the (June 30) deadline."
Damascus has blamed delays on security problems and the threat of rebel attacks on convoys taking chemical weapons by road to the northern port of Latakia. It has requested additional armor and communications equipment.
But the United States and the United Nations, which is jointly overseeing the destruction program with the Organization for the Prohibition of Chemical Weapons, said last week Syria has all the equipment it needs to carry out the operation and should proceed as quickly as possible.